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All 16 posts Subject: amphetamine Please login to post Down

flipper
(Hive Bee)
08-20-03 08:50
No 454670
      amphetamine

I have read somewhere that the most common route that amphetamine chemists take in clandestine labs is Number 3.

I found this in Synthetic Reductions in Clandestine Amphetamine and Methamphetamine Laboratories: A Review (https://www.rhodium.ws/chemistry/amphetamine.reduction.html)

And with these refs:
1: Pd/C
Nitrile reduction to phenethylamines
W.H. Hartung, Catalytic reduction of nitriles and oximes. J. Am. Chem. Soc., 50 (1928) 3370-3374. C.A. 23: 599 (1929).

2: Ni-Al, Figure 3.
Oxime reduced to amphetamine
J.W. Wilson, Synthesis of dl-amphetamine sulfate labeled with C14. J. Am. Pharm. Assoc., (Sci. Ed.), 39 (1950) 687. C.A. 45: 1728d (1951).

3: Ni-Al, Figure 3.
Oxime reduced to amphetamine
T. Kametani and Y. Nomura, reduction of nitrogen compounds by Raney nickel alloy and alkalai solution. I. J. Parm. Soc. Jpn., 74 (1954) 413-416. C.A. 49: 5342d (1955).

4: Ni-Al, Figure 3.
Oxime reduction to amphetamine
H.B. Hass, A.G. Susie and B.L. Heider, Nitroalkane derivatives. J. Org. Chem., 15 (1949) 8-14. C.A. 44: 4412d (1950).

5: Na/Alc, Figure 3.
Oxime reduction to amphetamine
F.M. Jaeger and J.A. van Dijk, Preparation of 2-phenylisopropylamine. Proc. Acad. Sci. Amsterdam, 44 (1941) 26-40. C.A. 37: 6219 (1943).

6: Na/Alc, Figure 3.
Oxime reduced to amphetamine
W. Leithe, Configuration of ephedrine bases. Berichte, 65 (1932) 660-666. C.A. 26: 3495 (1932).

7: Na-Hg, Figure 3.
Oxime reduced to amphetamine
D.H. Hey, dl-Phenylisopropylamine and related compounds. J. Chem. Soc. (1930) 18-21. C.A. 24: 1851 (1930).

8: LiAlH4, Figure 3.
Oxime reduced to amphetamine
K. Kotera, T. Okada and S. Miyazaki, Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates. Tetrahedron, 24 (1968) 5677-5690. C.A. 69: 67158a (1968).

afortunatly I don't have excess to these.

What yield can I expect from an normal low-pressure hydrogenation of P2P with NH2OH?

Osmium
(Stoni's sexual toy)
08-20-03 09:34
No 454676
User Picture       > I have read somewhere that the most ...

> I have read somewhere that the most common route that
> amphetamine chemists take in clandestine labs is Number 3.

That might have been the case in the 70s and early eighties, or maybe it's just a rumour.
If you have P2P and want to start producing amphetamine on a somewhat bigger scale (why? make meth!) then why bother creating the oxime first when you have to reduce it anyway?
For a bigger scale synth operation it makes more sense to do a catalytic hydrogenation with NH3. That of course is different when it comes to hobby chemistry.

> What yield can I expect from an normal low-pressure
> hydrogenation of P2P with NH2OH?

Oxime formation is nearly quantitative, the oxime reduction probably 80% or so. Just guessing.

I'm not fat just horizontally disproportionate.
http://www.whatreallyhappened.com

hypo
(Hive Addict)
08-20-03 10:05
No 454680
      nearly is relative ;)

Post 319296 (Rhodium: "P2P oxime in quantitative yield", Novel Discourse)

n'importe quoi

Rhodium
(Chief Bee)
08-20-03 11:48
No 454690
User Picture       Here's some of the references
(Rated as: good read)

Ref #1: Post 450229 (Rhodium: "Catalytic Reduction of Nitriles and Oximes", Methods Discourse)

Ref #4:
Nitroalkene Derivatives
H.B. Hass, A.G. Susie, B.L. Heider
J. Org. Chem. 15, 8-14 (1949) (https://www.rhodium.ws/pdf/nitro.alkene.derivatives.pdf)

Ref #7: Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants)

flipper
(Hive Bee)
08-21-03 10:35
No 454836
      Many many

Many many thanks. That will definatly help. Thanks.

Rhodium
(Chief Bee)
08-21-03 12:08
No 454846
User Picture       Here are a few of the references located
(Rated as: excellent)

Ref #1: Post 450229 (Rhodium: "Catalytic Reduction of Nitriles and Oximes", Methods Discourse)

Ref #3:
Reduction of nitrogen compounds by Raney nickel alloy and alkali solution. I.
T. Kametani and Y. Nomura
J. Pharm. Soc. Jpn. 74, 413-416(1954) (https://www.rhodium.ws/djvu/kametani.djvu)

Ref #4:
Nitroalkene Derivatives
H.B. Hass, A.G. Susie, B.L. Heider
J. Org. Chem. 15, 8-14 (1949) (https://www.rhodium.ws/pdf/nitro.alkene.derivatives.pdf)

Ref #6:
Configuration of ephedrine bases
W. Leithe
Chem. Ber. 65, 660-666 (1932) (https://www.rhodium.ws/djvu/leithe.djvu)

Ref #7: Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants)

Ref #8:
Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates
K. Kotera, T. Okada and S. Miyazaki
Tetrahedron 24, 5677-5690 (1968) (https://www.rhodium.ws/pdf/lah.oxime.reduction.aziridines.pdf)

Abstract
Separation of syn- and anti-isomers of aralkyl alkyl ketoximes and their tosylates has been carried out using 1-phenylpropan-2-one and 1--naphthylpropan-2-one. With the established configurations, LAH reduction of the oximes and their tosylates has been performed and the products have been analysed by GLC. The results clearly indicate that aziridine formation is strongly influenced by the configurations of the oximes and the oxime tosylates used.

Now only #2 and #5 are lacking...

Rhodium
(Chief Bee)
08-21-03 13:08
No 454857
User Picture       I knew I had a copy of this article somewhere...
(Rated as: excellent)

Ref #8:

Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates
K. Kotera, T. Okada and S. Miyazaki
Tetrahedron 24, 5677-5690 (1968) (https://www.rhodium.ws/pdf/lah.oxime.reduction.aziridines.pdf)

Abstract

Separation of syn- and anti-isomers of aralkyl alkyl ketoximes and their tosylates has been carried out using 1-phenylpropan-2-one and 1--naphthylpropan-2-one. With the established configurations, LAH reduction of the oximes and their tosylates has been performed and the products have been analysed by GLC. The results clearly indicate that aziridine formation is strongly influenced by the configurations of the oximes and the oxime tosylates used.

Now only #2 and #5 are lacking...

catfish
(Hive Bee)
08-22-03 10:12
No 455007
      cheesy but ....

Hi all-
L. Krasnec, Z. Chem., 11, 110, (1971); Synthesis, 53 (1972) is all I could dig up at home. They may have applications...
I have a few more, but they're real old (I'm working with a 1977 edition, so bear with me).
-cfg

all information related for educational purposes only!
no quarter asked, none given

flipper
(Hive Bee)
08-27-03 14:56
No 455992
      So if SWIM has Benzedrine how does he make...

So if SWIM has Benzedrine how does he make Dexedrine of it.

Is this a good way to do it:

Rusznak et al., Resolution of Phenylisopropylamines, Hung. Teljes, 12,208 (Cl.C07B), 28 Sep. 1976, Appl. 1,516, 08 Nov. 1974; C.A. 85: 192337q, p. 518 (1976).

Phenylisopropylamines and phenylisopropylmethylamines and various substituted amines were resolved with 0.5 mole tartaric acid in benzene-water containing 0.5 mole sodium hydroxide or potassium hydroxide by selective extraction of either enantiomer.

A mixture of 0.1 mole (13.52 g.) phenylisopropylamine (or 14.92 g. methamphetamine base) in 60 ml benzene, 0.05 mole d-tartaric acid (7.50 g.) in 30 ml water, and 2 g sodium hydroxide (reagent grade or titrated equivalent) in 3 ml water was kept 4 hours with intermittent shaking, and the organic phase evaporated to give 98% L-phenylisopropylamine. The aqueous phase was extracted with benzene at pH 13 and evaporated to give 96% D-enantiomer. From Procedures for the Resolution of Racemic Amphetamines (https://www.rhodium.ws/chemistry/amphetamine.resolution.html)

Or if SWIM wan't make Dex should do it with another method like this one. Preparation of Optically pure Amphetamines by the way of alpha-Methylhydrocinnamic Acid (https://www.rhodium.ws/chemistry/alpha-methylhydrocinnamic.html)

Aurelius
(Active Asperger Archivist)
08-29-03 02:49
No 456273
      How do you miss these?

Post 422067 (Aurelius: "Ephedrine Compilation", Stimulants)

An entire section racemization and an entire section of resolution. Plus,....

Post 408293 (Rhodium: "The Stimulants Forum FAQ", Stimulants)

This has links to the same type of information.

Act quickly or not at all.

flipper
(Hive Bee)
09-01-03 09:42
No 456701
      oxime question

In post Post 319296 (Rhodium: "P2P oxime in quantitative yield", Novel Discourse) they use 5 grams of calcium oxide and in post Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants) they use NaOH.

When I look at some patents I notice they don't use anything. Just the stuff they gonna make the oxime off and the HydroxylAmine. And if they use something extra it is an acid, like formic acid. See Method of manufacturing high purity oximes from aqueous hydroxylamine and ketones US 6235935 (http://l2.espacenet.com/dips/viewer?PN=US6235935&CY=gb&LG=en&DB=EPD).

So why is with P2P calcium oxide or NaOH used?

The reason why I ask this is that when SWIM wants to do a 2 kilo batch he need 10 kilos of calcium oxide. And that's way to much.

These are my questions:

So why is with P2P, calcium oxide or NaOH used?
Can he when he is doing a 2 kilo batch use 5 kilos Calcium oxide instead of 10 kilos?
And what would happen when he uses no Calcium Oxide?
Can you do this in a microwave?

flipper
09-04-03 09:18
      Can somebody please help me with these ...
(Rated as: redundant)

flipper
09-05-03 22:43
      please :-S
(Rated as: redundant)

Vitus_Verdegast
(Hive Bee)
09-06-03 02:21
No 457407
User Picture       No spoonfeeding for you, mister! ;-)

!!!!!! mad mad mad

Now you are really asking to be spoonfed. Read up on the reaction mechanism, you don't have to be a genius for that. Ask yourself this question: How is an oxime formed?

However, since you used the magic word, I'll give you a hint:

Amines form salts with acids

A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)

flipper
09-06-03 17:32
      thanks
(Rated as: insignificant)

Vitus_Verdegast
(Hive Bee)
09-06-03 18:19
No 457485
User Picture       I'm not kidding

You should learn to look up such basic chemistry yourself in an org chem textbook, or on various webpages, eg. look at LaBTop's sticky threads in the methods and newbee forum, they are not there only for decoration!!! shocked mad

I can't believe you waited 5 days for someone to answer your questions, when you could have found them easily in 5 minutes.

Don't be so lazy, pick up a book (or click on a link)!! mad

A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)

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	All 16 posts		Subject: amphetamine		Please login to post		Down


		flipper (Hive Bee) 08-20-03 08:50 No 454670				amphetamine
						I have read somewhere that the most common route that amphetamine chemists take in clandestine labs is Number 3. I found this in Synthetic Reductions in Clandestine Amphetamine and Methamphetamine Laboratories: A Review (https://www.rhodium.ws/chemistry/amphetamine.reduction.html) And with these refs: 1: Pd/C Nitrile reduction to phenethylamines W.H. Hartung, Catalytic reduction of nitriles and oximes. J. Am. Chem. Soc., 50 (1928) 3370-3374. C.A. 23: 599 (1929). 2: Ni-Al, Figure 3. Oxime reduced to amphetamine J.W. Wilson, Synthesis of dl-amphetamine sulfate labeled with C14. J. Am. Pharm. Assoc., (Sci. Ed.), 39 (1950) 687. C.A. 45: 1728d (1951). 3: Ni-Al, Figure 3. Oxime reduced to amphetamine T. Kametani and Y. Nomura, reduction of nitrogen compounds by Raney nickel alloy and alkalai solution. I. J. Parm. Soc. Jpn., 74 (1954) 413-416. C.A. 49: 5342d (1955). 4: Ni-Al, Figure 3. Oxime reduction to amphetamine H.B. Hass, A.G. Susie and B.L. Heider, Nitroalkane derivatives. J. Org. Chem., 15 (1949) 8-14. C.A. 44: 4412d (1950). 5: Na/Alc, Figure 3. Oxime reduction to amphetamine F.M. Jaeger and J.A. van Dijk, Preparation of 2-phenylisopropylamine. Proc. Acad. Sci. Amsterdam, 44 (1941) 26-40. C.A. 37: 6219 (1943). 6: Na/Alc, Figure 3. Oxime reduced to amphetamine W. Leithe, Configuration of ephedrine bases. Berichte, 65 (1932) 660-666. C.A. 26: 3495 (1932). 7: Na-Hg, Figure 3. Oxime reduced to amphetamine D.H. Hey, dl-Phenylisopropylamine and related compounds. J. Chem. Soc. (1930) 18-21. C.A. 24: 1851 (1930). 8: LiAlH4, Figure 3. Oxime reduced to amphetamine K. Kotera, T. Okada and S. Miyazaki, Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates. Tetrahedron, 24 (1968) 5677-5690. C.A. 69: 67158a (1968). afortunatly I don't have excess to these. What yield can I expect from an normal low-pressure hydrogenation of P2P with NH2OH?



		Osmium (Stoni's sexual toy) 08-20-03 09:34 No 454676				> I have read somewhere that the most ...
						> I have read somewhere that the most common route that > amphetamine chemists take in clandestine labs is Number 3. That might have been the case in the 70s and early eighties, or maybe it's just a rumour. If you have P2P and want to start producing amphetamine on a somewhat bigger scale (why? make meth!) then why bother creating the oxime first when you have to reduce it anyway? For a bigger scale synth operation it makes more sense to do a catalytic hydrogenation with NH3. That of course is different when it comes to hobby chemistry. > What yield can I expect from an normal low-pressure > hydrogenation of P2P with NH2OH? Oxime formation is nearly quantitative, the oxime reduction probably 80% or so. Just guessing. I'm not fat just horizontally disproportionate. http://www.whatreallyhappened.com



		hypo (Hive Addict) 08-20-03 10:05 No 454680				nearly is relative ;)
						Post 319296 (Rhodium: "P2P oxime in quantitative yield", Novel Discourse) n'importe quoi



		Rhodium (Chief Bee) 08-20-03 11:48 No 454690				Here's some of the references (Rated as: good read)
						Ref #1: Post 450229 (Rhodium: "Catalytic Reduction of Nitriles and Oximes", Methods Discourse) Ref #4: Nitroalkene Derivatives H.B. Hass, A.G. Susie, B.L. Heider J. Org. Chem. 15, 8-14 (1949) (https://www.rhodium.ws/pdf/nitro.alkene.derivatives.pdf) Ref #7: Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants)



		flipper (Hive Bee) 08-21-03 10:35 No 454836				Many many
						Many many thanks. That will definatly help. Thanks.



		Rhodium (Chief Bee) 08-21-03 12:08 No 454846				Here are a few of the references located (Rated as: excellent)
						Ref #1: Post 450229 (Rhodium: "Catalytic Reduction of Nitriles and Oximes", Methods Discourse) Ref #3: Reduction of nitrogen compounds by Raney nickel alloy and alkali solution. I. T. Kametani and Y. Nomura J. Pharm. Soc. Jpn. 74, 413-416(1954) (https://www.rhodium.ws/djvu/kametani.djvu) Ref #4: Nitroalkene Derivatives H.B. Hass, A.G. Susie, B.L. Heider J. Org. Chem. 15, 8-14 (1949) (https://www.rhodium.ws/pdf/nitro.alkene.derivatives.pdf) Ref #6: Configuration of ephedrine bases W. Leithe Chem. Ber. 65, 660-666 (1932) (https://www.rhodium.ws/djvu/leithe.djvu) Ref #7: Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants) Ref #8: Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates K. Kotera, T. Okada and S. Miyazaki Tetrahedron 24, 5677-5690 (1968) (https://www.rhodium.ws/pdf/lah.oxime.reduction.aziridines.pdf) Abstract Separation of syn- and anti-isomers of aralkyl alkyl ketoximes and their tosylates has been carried out using 1-phenylpropan-2-one and 1--naphthylpropan-2-one. With the established configurations, LAH reduction of the oximes and their tosylates has been performed and the products have been analysed by GLC. The results clearly indicate that aziridine formation is strongly influenced by the configurations of the oximes and the oxime tosylates used. Now only #2 and #5 are lacking...



		Rhodium (Chief Bee) 08-21-03 13:08 No 454857				I knew I had a copy of this article somewhere... (Rated as: excellent)
						Ref #8: Stereochemistry of aziridine formation by reduction of oximes with lithium aluminum hydride on arylalkyl alkyl ketoximes and their tosylates K. Kotera, T. Okada and S. Miyazaki Tetrahedron 24, 5677-5690 (1968) (https://www.rhodium.ws/pdf/lah.oxime.reduction.aziridines.pdf) Abstract Separation of syn- and anti-isomers of aralkyl alkyl ketoximes and their tosylates has been carried out using 1-phenylpropan-2-one and 1--naphthylpropan-2-one. With the established configurations, LAH reduction of the oximes and their tosylates has been performed and the products have been analysed by GLC. The results clearly indicate that aziridine formation is strongly influenced by the configurations of the oximes and the oxime tosylates used. Now only #2 and #5 are lacking...



		catfish (Hive Bee) 08-22-03 10:12 No 455007				cheesy but ....
						Hi all- L. Krasnec, Z. Chem., 11, 110, (1971); Synthesis, 53 (1972) is all I could dig up at home. They may have applications... I have a few more, but they're real old (I'm working with a 1977 edition, so bear with me). -cfg all information related for educational purposes only! no quarter asked, none given



		flipper (Hive Bee) 08-27-03 14:56 No 455992				So if SWIM has Benzedrine how does he make...
						So if SWIM has Benzedrine how does he make Dexedrine of it. Is this a good way to do it: Rusznak et al., Resolution of Phenylisopropylamines, Hung. Teljes, 12,208 (Cl.C07B), 28 Sep. 1976, Appl. 1,516, 08 Nov. 1974; C.A. 85: 192337q, p. 518 (1976). Phenylisopropylamines and phenylisopropylmethylamines and various substituted amines were resolved with 0.5 mole tartaric acid in benzene-water containing 0.5 mole sodium hydroxide or potassium hydroxide by selective extraction of either enantiomer. A mixture of 0.1 mole (13.52 g.) phenylisopropylamine (or 14.92 g. methamphetamine base) in 60 ml benzene, 0.05 mole d-tartaric acid (7.50 g.) in 30 ml water, and 2 g sodium hydroxide (reagent grade or titrated equivalent) in 3 ml water was kept 4 hours with intermittent shaking, and the organic phase evaporated to give 98% L-phenylisopropylamine. The aqueous phase was extracted with benzene at pH 13 and evaporated to give 96% D-enantiomer. From Procedures for the Resolution of Racemic Amphetamines (https://www.rhodium.ws/chemistry/amphetamine.resolution.html) Or if SWIM wan't make Dex should do it with another method like this one. Preparation of Optically pure Amphetamines by the way of alpha-Methylhydrocinnamic Acid (https://www.rhodium.ws/chemistry/alpha-methylhydrocinnamic.html)



		Aurelius (Active Asperger Archivist) 08-29-03 02:49 No 456273				How do you miss these?
						Post 422067 (Aurelius: "Ephedrine Compilation", Stimulants) An entire section racemization and an entire section of resolution. Plus,.... Post 408293 (Rhodium: "The Stimulants Forum FAQ", Stimulants) This has links to the same type of information. Act quickly or not at all.



		flipper (Hive Bee) 09-01-03 09:42 No 456701				oxime question
						In post Post 319296 (Rhodium: "P2P oxime in quantitative yield", Novel Discourse) they use 5 grams of calcium oxide and in post Post 402025 (Rhodium: "Ye olde Benzedrine", Stimulants) they use NaOH. When I look at some patents I notice they don't use anything. Just the stuff they gonna make the oxime off and the HydroxylAmine. And if they use something extra it is an acid, like formic acid. See Method of manufacturing high purity oximes from aqueous hydroxylamine and ketones US 6235935 (http://l2.espacenet.com/dips/viewer?PN=US6235935&CY=gb&LG=en&DB=EPD). So why is with P2P calcium oxide or NaOH used? The reason why I ask this is that when SWIM wants to do a 2 kilo batch he need 10 kilos of calcium oxide. And that's way to much. These are my questions: So why is with P2P, calcium oxide or NaOH used? Can he when he is doing a 2 kilo batch use 5 kilos Calcium oxide instead of 10 kilos? And what would happen when he uses no Calcium Oxide? Can you do this in a microwave?



		flipper 09-04-03 09:18				Can somebody please help me with these ... (Rated as: redundant)



		flipper 09-05-03 22:43				please :-S (Rated as: redundant)



		Vitus_Verdegast (Hive Bee) 09-06-03 02:21 No 457407				No spoonfeeding for you, mister! ;-)
						!!!!!! Now you are really asking to be spoonfed. Read up on the reaction mechanism, you don't have to be a genius for that. Ask yourself this question: How is an oxime formed? However, since you used the magic word, I'll give you a hint: Amines form salts with acids A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)



		flipper 09-06-03 17:32				thanks (Rated as: insignificant)



		Vitus_Verdegast (Hive Bee) 09-06-03 18:19 No 457485				I'm not kidding
						You should learn to look up such basic chemistry yourself in an org chem textbook, or on various webpages, eg. look at LaBTop's sticky threads in the methods and newbee forum, they are not there only for decoration!!! I can't believe you waited 5 days for someone to answer your questions, when you could have found them easily in 5 minutes. Don't be so lazy, pick up a book (or click on a link)!! A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)

All 16 posts	End of thread	Top