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All 9 posts Subject: Phenylacetone Please login to post Down

ocoward
(Stranger)
02-17-03 05:38
No 408792
      Phenylacetone

Is Phenylacetone used in photography or film processing? I think I remember hearing about the above being used in black and white film or processing thereof. If there is something you may know of outside the scope of this question, please expand. Thanks.

terbium
(Old P2P Cook)
02-17-03 05:59
No 408803
      P2P

As you were told just a couple of days ago, in the US, P2P is a Schedule 1 Controlled Substance. It is not used in photography, film processing, pest control or any other consumer or industrial application because it is a Schedule 1 Controlled Substance. You will not find any cover story or scam that will enable you to purchase a Schedule 1 Controlled Substance such as P2P.

Piperidine has at times been used in commercial film processing but piperidine is only usefull if you wish to manufacture PCP.

All those moments will be lost in time, like tears in rain.

littlejasebee
02-17-03 06:23
      I like having old p2p cooks around here
(Rated as: insignificant)

yellium
(I'm Yust a Typo)
02-17-03 07:08
No 408825
      2,5-DMA is also used in the photographic ...

2,5-DMA is also used in the photographic industry but that's only interesting if you're into heavy duty psychedelics.

terbium
(Old P2P Cook)
02-17-03 07:41
No 408838
      2,5-DMA

But it is a mystery as to who is using the 2,5-DMA and for what. Even Shulgin says that he doesn't know.

All those moments will be lost in time, like tears in rain.

Rhodium
(Chief Bee)
02-17-03 09:13
No 408858
User Picture       P2P in photo supplies

https://www.rhodium.ws/chemistry/chickenfeed.html (Fourth paragraph under the "background" heading)

zorohydride
(Stranger)
02-22-03 16:04
No 410768
      Here's my favorite BULK synthesis
(Rated as: good read)

From one old cook to another. Into a crock is added 1 gallon of refrigerated (substituted) PhCH₂CN and two gallons of 25% Sodium Methoxide and they are stirred together for 10 minutes. Now add 1 gallon of Ethyl Acetate; stir and warm to 60°C for about 2 hr and crops of crystals form [no crystals means a big failure]. The origonal Gillman-Blatt V3 calls for ether to help precipitate and wash, so use today Diglyme. Filter on a poly table top buchner and wash with more solvent to remove as much starting materials as they will corrupt your final product! Allow to dry. You now have sodium salt of the α-acetyl-acetonitrile. Bung your salt at a rate of 1 lb into 2 pt of 40% Sulfuric with rapid stirring and continue until effervescence [hydrolysis and subsequent decarboxylation of the nitrile], now turn on the heat and stir rapidly; add enough water to make a 20% acid solution and you will see an organic layer form. The ETA is about 2 hr. Wash with water and dilute bicarb.

Bozakium
(Hive Addict)
07-30-04 17:06
No 522724
      Bulk Synthesis Correction
(Rated as: good read)

Decant the supernatant liquid! You forgot to decant the supernatant liquid! Fools! Fools!
Here's the original synth, with all the details as it appeared in the Journal Bibliothek fur chemie von der Fremdenverkersburo:
(Proper German-English translation by Bozakium)
To a 25 litre crock nestled in a dry ice/acetone bath is introduced 4 litres of liquid(substituted) BzCN dimer. Dropwise with stirring 8 litres of equimolar (25.223%) sodium methylate in anhydrous acetone is added. The stirring is continued until all the emulsion disappears into solution.Allow to stand until no more emulsion forms, stirring each time to disperse it. Add 4 litres of cooled ethyl acetate as a co-solvent. Remove from the dry-ice bath and allow to warm to room temperature. At room temp(20C), the solution will be seen to separate ito two separate, but hard to see layers. Decant the supernatant liquid and discard it. This will pollute the product if allowed to remain,as it contains many Bz2 moieties which will thrust their way into the crystal lattices; however the small amount (<50mL) left behind actually helps catalyze the crystallization. This is why we decant.
Warm slowly (10-15C/Hr), with stirring to 60C. Crystallization will commence at 55-58C and cease before 62C. Any wider a range indicates a polluted product or improper stoichiometry.Collect accordingly. Be sure to use the BzCn dimer, as even with adjusted stoichiometry, the momomer is unstable and will cause polymerization in the end product (sticky goo). Gillmann /Blatt (1903) used (monoisobutyl)ether to assist forcing crystallization, but diglyme is found to be better as it does not tend to force dirty crystals against their will as does ether. Vacuum filter through a #69(really)Buchner funnel with 120-bore or smaller escrima paper. Drying may be done at STP, but is aided by a combination infrared/ultraviolet heat lamp. Do not use a regular light bulb, as excessive photons in the 589 to 589.4 nM wavelength range(yellow) excite the electrons on the androgyne carbon of the alpha-acetyl group and can cause explosive decomposition. Keep this intermediate out of direct sunlight for the same reason. Failing to decant the supernatant liquid in the earlier step GREATLY exacerbates this danger! The white, needle-like prisms(other crystals indicate failure, an incorrect product)are the sodium salt of n-acetylacetonitrile. Bung the salt at a rate of 450g /500mL of 40%(by wt. not vol.) sulfuric acid in a large beaker with rapid stirring. "Bung" translates best into "refresh, with shooshing", this is done in practice as one would spread rock salt on an icy sidewalk out of a scoop, with sweeping horizontal motion. I believe it is to allow the reaction with the sulfuric to proceed upon maximum unimpeded surface area, to prevent diphenylacetone formation. Stir rapidly during bunging to break up the effervescence(or beaker will overflow), until all effervescence(you should see the German word for that!) ceases. Proto- and final hydrolysis as well as the subsequent decarboxylation should now be complete. Check by TLC eluted with 60/40 tin/lead dichromate(at 2% wt/vol dilution in deionized, distilled dihydrogen oxide. Develop the plates with iodine vapour to visualize. If not complete, a SMALL amount of concentrated acid may be added dropwise wit very fast strring, rechecking TLC after every .22 drops/mole of crystals used. Heat on an electric mantle(NO flame), with rapid stirring to 75C for one hour to allow deracemization.
Add water to an acidity of 20%, checking with pH paper. The organic layer containing the product will float. Extract with light petroleum(pentanes), wash 3x with a 10% sodium bicarbonate solution. Eveporate the solvent in vacuo. Yield should be 80-90%. Mp should be +/- 2 deg. of reference product. Total synthesis time(minus workup) is ca. 2 Hr. This is a pretty small-caliber synthesis and should be easy for anyone to compleat sucessfully.

sheake_me
(Stranger)
11-06-04 11:10
No 540019
      and the end product is P2P

Tank you for posting this whole synth in such a friendly manner but just to bee certain the end product is p2p?

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	All 9 posts		Subject: Phenylacetone		Please login to post		Down


		ocoward (Stranger) 02-17-03 05:38 No 408792				Phenylacetone
						Is Phenylacetone used in photography or film processing? I think I remember hearing about the above being used in black and white film or processing thereof. If there is something you may know of outside the scope of this question, please expand. Thanks.



		terbium (Old P2P Cook) 02-17-03 05:59 No 408803				P2P
						As you were told just a couple of days ago, in the US, P2P is a Schedule 1 Controlled Substance. It is not used in photography, film processing, pest control or any other consumer or industrial application because it is a Schedule 1 Controlled Substance. You will not find any cover story or scam that will enable you to purchase a Schedule 1 Controlled Substance such as P2P. Piperidine has at times been used in commercial film processing but piperidine is only usefull if you wish to manufacture PCP. All those moments will be lost in time, like tears in rain.



		littlejasebee 02-17-03 06:23				I like having old p2p cooks around here (Rated as: insignificant)



		yellium (I'm Yust a Typo) 02-17-03 07:08 No 408825				2,5-DMA is also used in the photographic ...
						2,5-DMA is also used in the photographic industry but that's only interesting if you're into heavy duty psychedelics.



		terbium (Old P2P Cook) 02-17-03 07:41 No 408838				2,5-DMA
						But it is a mystery as to who is using the 2,5-DMA and for what. Even Shulgin says that he doesn't know. All those moments will be lost in time, like tears in rain.



		Rhodium (Chief Bee) 02-17-03 09:13 No 408858				P2P in photo supplies
						https://www.rhodium.ws/chemistry/chickenfeed.html (Fourth paragraph under the "background" heading)



		zorohydride (Stranger) 02-22-03 16:04 No 410768				Here's my favorite BULK synthesis (Rated as: good read)
						From one old cook to another. Into a crock is added 1 gallon of refrigerated (substituted) PhCH₂CN and two gallons of 25% Sodium Methoxide and they are stirred together for 10 minutes. Now add 1 gallon of Ethyl Acetate; stir and warm to 60°C for about 2 hr and crops of crystals form [no crystals means a big failure]. The origonal Gillman-Blatt V3 calls for ether to help precipitate and wash, so use today Diglyme. Filter on a poly table top buchner and wash with more solvent to remove as much starting materials as they will corrupt your final product! Allow to dry. You now have sodium salt of the α-acetyl-acetonitrile. Bung your salt at a rate of 1 lb into 2 pt of 40% Sulfuric with rapid stirring and continue until effervescence [hydrolysis and subsequent decarboxylation of the nitrile], now turn on the heat and stir rapidly; add enough water to make a 20% acid solution and you will see an organic layer form. The ETA is about 2 hr. Wash with water and dilute bicarb.



		Bozakium (Hive Addict) 07-30-04 17:06 No 522724				Bulk Synthesis Correction (Rated as: good read)
						Decant the supernatant liquid! You forgot to decant the supernatant liquid! Fools! Fools! Here's the original synth, with all the details as it appeared in the Journal Bibliothek fur chemie von der Fremdenverkersburo: (Proper German-English translation by Bozakium) To a 25 litre crock nestled in a dry ice/acetone bath is introduced 4 litres of liquid(substituted) BzCN dimer. Dropwise with stirring 8 litres of equimolar (25.223%) sodium methylate in anhydrous acetone is added. The stirring is continued until all the emulsion disappears into solution.Allow to stand until no more emulsion forms, stirring each time to disperse it. Add 4 litres of cooled ethyl acetate as a co-solvent. Remove from the dry-ice bath and allow to warm to room temperature. At room temp(20C), the solution will be seen to separate ito two separate, but hard to see layers. Decant the supernatant liquid and discard it. This will pollute the product if allowed to remain,as it contains many Bz2 moieties which will thrust their way into the crystal lattices; however the small amount (<50mL) left behind actually helps catalyze the crystallization. This is why we decant. Warm slowly (10-15C/Hr), with stirring to 60C. Crystallization will commence at 55-58C and cease before 62C. Any wider a range indicates a polluted product or improper stoichiometry.Collect accordingly. Be sure to use the BzCn dimer, as even with adjusted stoichiometry, the momomer is unstable and will cause polymerization in the end product (sticky goo). Gillmann /Blatt (1903) used (monoisobutyl)ether to assist forcing crystallization, but diglyme is found to be better as it does not tend to force dirty crystals against their will as does ether. Vacuum filter through a #69(really)Buchner funnel with 120-bore or smaller escrima paper. Drying may be done at STP, but is aided by a combination infrared/ultraviolet heat lamp. Do not use a regular light bulb, as excessive photons in the 589 to 589.4 nM wavelength range(yellow) excite the electrons on the androgyne carbon of the alpha-acetyl group and can cause explosive decomposition. Keep this intermediate out of direct sunlight for the same reason. Failing to decant the supernatant liquid in the earlier step GREATLY exacerbates this danger! The white, needle-like prisms(other crystals indicate failure, an incorrect product)are the sodium salt of n-acetylacetonitrile. Bung the salt at a rate of 450g /500mL of 40%(by wt. not vol.) sulfuric acid in a large beaker with rapid stirring. "Bung" translates best into "refresh, with shooshing", this is done in practice as one would spread rock salt on an icy sidewalk out of a scoop, with sweeping horizontal motion. I believe it is to allow the reaction with the sulfuric to proceed upon maximum unimpeded surface area, to prevent diphenylacetone formation. Stir rapidly during bunging to break up the effervescence(or beaker will overflow), until all effervescence(you should see the German word for that!) ceases. Proto- and final hydrolysis as well as the subsequent decarboxylation should now be complete. Check by TLC eluted with 60/40 tin/lead dichromate(at 2% wt/vol dilution in deionized, distilled dihydrogen oxide. Develop the plates with iodine vapour to visualize. If not complete, a SMALL amount of concentrated acid may be added dropwise wit very fast strring, rechecking TLC after every .22 drops/mole of crystals used. Heat on an electric mantle(NO flame), with rapid stirring to 75C for one hour to allow deracemization. Add water to an acidity of 20%, checking with pH paper. The organic layer containing the product will float. Extract with light petroleum(pentanes), wash 3x with a 10% sodium bicarbonate solution. Eveporate the solvent in vacuo. Yield should be 80-90%. Mp should be +/- 2 deg. of reference product. Total synthesis time(minus workup) is ca. 2 Hr. This is a pretty small-caliber synthesis and should be easy for anyone to compleat sucessfully.



		sheake_me (Stranger) 11-06-04 11:10 No 540019				and the end product is P2P
						Tank you for posting this whole synth in such a friendly manner but just to bee certain the end product is p2p?

All 9 posts	End of thread	Top