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All 6 posts Subject: A route to P2P Please login to post Down

Deathwish
(Stranger)
05-09-00 02:51
No 1615
      A route to P2P

While purusing my gleaning from web searches I came across this reaction. This was taken from an old Hive posting by Everyman who plagarized it from an older posting between Rhodium and Drone 342. The link to the prior post does not produce anything, nor does the post go into detail regarding the specifics of this reaction. Was just wondering if anyone had any more info on this.

Toluene + Cl2(gas) --> Benzyl chloride
Acetic Acid + SO4(gas) -->acetic anhydride
Benz.Chlor. +Acetic Anhydride --->via Electrolysis ---> P2P

A pondersome Deathwish...

Deathwish
(Stranger)
05-09-00 04:14
No 1648
      Re: A route to P2P

The most noteworthy aspect of this reaction, which I dont know if anyone noticed, is that it provides a route to Meth w/o Psuedo(E). Wether this is entirely workable might be problematic. I leave that up to more experienced out there.

Deathwish

WizardX
(Wizard Master)
05-09-00 06:35
No 1707
User Picture       Re: A route to P2P
(Rated as: excellent)

Yes the reaction is workable, however not as easy as you may think. The P2P synthesis from benzyl chloride + Acetic Anhydride is one that gives good results with a skilled operator.

P2P Synthesis via electrosynthesis of ketones.

Tetrahedron Letters, 27(35), 4175-4176 (1986)
DOI:10.1016/S0040-4039(00)84940-0

Patent EP198743 Process for the electrosynthesis of ketones.
Patent US4629541 Process for the electrosynthesis of ketones.

30 mmoles of Benzyl Chloride (3.79g), an excess of Acetic Anhydride (>3.5g) and either 1 mmol Tetrabutylammonium Iodide (0.37g) or 1 mmol tetrafluoroborate (0.09g) are dissolved in 25ml of DMF.

This is transferred to an Electrolytic Cell with the anode being a rod of Magnesium (Mg) or Duralin (Al) (1 cm diameter) and the cathode being a cylindrical grid of Stainless Steel or Nickel. The cell is immersed in an ice-water bath so that the temp stays between 0-10°C. A constant current intensity (0.4 Amperes) is applied until 3 to 4 moles of electrons per mole of Benzyl Chloride (in this case 90-120 mmoles) are passed.

The contents of the cell are transferred to a flask and refluxed with 20% H₂SO₄ for 1 hr in order to destroy the excess of Acetic Anhydride and release the ketone from the enol ester which may be formed.

The mixture is then extracted several times with ether (or other non-polar solvent?), and the extract is vacuum distilled.

CHEMMAN
(Stranger)
05-09-00 11:40
No 1782
      Re: A route to P2P

I am in a position for both helping and getting helped here. I have both the precursors on hand, and am about to play with the cell.Get one cell working , and dont even try to scale it up.Make say 6 of the fuchers in parallel with an overhead bussbar and a suitable powersupply.My trade is electronics, so that bit is not a problem.Anyone in the same position??

ozbee
(Stranger)
05-09-00 12:46
No 1797
      Re: A route to P2P

Hi CHEMMAN
You won't believe what info ozbee has gained for us . We need to have a bit of a personal chat about this . Do you have the time ? I think I may have a better alternative for knocking up some benzyl chloride , I have 3.5ltrs ready to use my friend . I wan't you to check out some wicked info on our ultimate Aussie plan . Lets go hush mate .

Backyard chemistry
down under with ozbee

encopo
(Hive Bee)
10-15-01 21:35
No 224915
      Re: A route to P2P

An easier way to make benzal chloride is shown in the
patent U.S. Pat.#1,280,612. Check out this excerpt from
a recent post of mine in serious chemistry:

"I've been looking around for a nice way to get some
benzaldehyde to use in this. looking at the
"phenylacetones.htm" file I found a patent reference
for the production of benzyl chloride by the chlorination
of toluene (it's the same thing as toluene with 1 xtra
Cl on the carbon outcrop).
The process bubbled Cl2 through Toluene, but it also said
that using "bleaching powder" at high temperature with
an acid provides nascent chlorine.
However, the guy who wrote this has a bitch about side
products. Now here is the NICE bit:
"I have discovered, however....,
by heating to a high temperature
an anhydrous mixture of toluene
and bleaching powder, with thorough
commingling, and without the use of
any acid, the chlorination of the
toluene is effected without any of
the disadvantages incident to the
processes above referred to. In
the absence of any added water the
chlorin from the bleaching powder
seems to go directly to produce
benzyl chlorid in the side chain
without attacking the nucleus, even
though the process is carried on in
the presence of iron, as in an
iron vessel"
Hmm. That looks nice. The reaction is pretty much:
Heat toluene to 90'C. Slowly add equal amount (weight)
of Ca(OCl)2 (pool shock), and raise temperature to
100'-105'C, leaving it there 1 hour or until reaction
complete. Settle. Decant of oil.
This oil contains 30-35% benzyl chloride and 65-70%
toluene.
However, We don't want benzyl chloride, do we? We want
BENZAL chloride. The patent goes on to describe that if
sufficient amount of Ca(OCl)2 is added, the toluene is
completely converted to Benzal Chloride and
Benzo Trichloride. Upon boiling in alkaline water, we
get Benzaldehyde and Benzoic acid. Voila.
Hope this will be a good addition to the home-brew-E
method, as many bees don't have that much benzaldehyde
lying around."

I assume that what you're after is BENZAL chloride,
but similiarly benzyl chloride and benzo trichloride
could be prepared as above. Just be careful that you're
reading BENZAL, not benzyl.

As to the info that OZBEE seems to have dug up, I would
be very interested in assisting in the exploration of this
field, plus the "otc-ination". PM me oz for discussion.
Don't mind me. I'm mentally ill.

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	All 6 posts		Subject: A route to P2P		Please login to post		Down


		Deathwish (Stranger) 05-09-00 02:51 No 1615				A route to P2P
						While purusing my gleaning from web searches I came across this reaction. This was taken from an old Hive posting by Everyman who plagarized it from an older posting between Rhodium and Drone 342. The link to the prior post does not produce anything, nor does the post go into detail regarding the specifics of this reaction. Was just wondering if anyone had any more info on this. Toluene + Cl2(gas) --> Benzyl chloride Acetic Acid + SO4(gas) -->acetic anhydride Benz.Chlor. +Acetic Anhydride --->via Electrolysis ---> P2P A pondersome Deathwish...



		Deathwish (Stranger) 05-09-00 04:14 No 1648				Re: A route to P2P
						The most noteworthy aspect of this reaction, which I dont know if anyone noticed, is that it provides a route to Meth w/o Psuedo(E). Wether this is entirely workable might be problematic. I leave that up to more experienced out there. Deathwish



		WizardX (Wizard Master) 05-09-00 06:35 No 1707				Re: A route to P2P (Rated as: excellent)
						Yes the reaction is workable, however not as easy as you may think. The P2P synthesis from benzyl chloride + Acetic Anhydride is one that gives good results with a skilled operator. P2P Synthesis via electrosynthesis of ketones. Tetrahedron Letters, 27(35), 4175-4176 (1986) DOI:10.1016/S0040-4039(00)84940-0 Patent EP198743 Process for the electrosynthesis of ketones. Patent US4629541 Process for the electrosynthesis of ketones. 30 mmoles of Benzyl Chloride (3.79g), an excess of Acetic Anhydride (>3.5g) and either 1 mmol Tetrabutylammonium Iodide (0.37g) or 1 mmol tetrafluoroborate (0.09g) are dissolved in 25ml of DMF. This is transferred to an Electrolytic Cell with the anode being a rod of Magnesium (Mg) or Duralin (Al) (1 cm diameter) and the cathode being a cylindrical grid of Stainless Steel or Nickel. The cell is immersed in an ice-water bath so that the temp stays between 0-10°C. A constant current intensity (0.4 Amperes) is applied until 3 to 4 moles of electrons per mole of Benzyl Chloride (in this case 90-120 mmoles) are passed. The contents of the cell are transferred to a flask and refluxed with 20% H₂SO₄ for 1 hr in order to destroy the excess of Acetic Anhydride and release the ketone from the enol ester which may be formed. The mixture is then extracted several times with ether (or other non-polar solvent?), and the extract is vacuum distilled.



		CHEMMAN (Stranger) 05-09-00 11:40 No 1782				Re: A route to P2P
						I am in a position for both helping and getting helped here. I have both the precursors on hand, and am about to play with the cell.Get one cell working , and dont even try to scale it up.Make say 6 of the fuchers in parallel with an overhead bussbar and a suitable powersupply.My trade is electronics, so that bit is not a problem.Anyone in the same position??



		ozbee (Stranger) 05-09-00 12:46 No 1797				Re: A route to P2P
						Hi CHEMMAN You won't believe what info ozbee has gained for us . We need to have a bit of a personal chat about this . Do you have the time ? I think I may have a better alternative for knocking up some benzyl chloride , I have 3.5ltrs ready to use my friend . I wan't you to check out some wicked info on our ultimate Aussie plan . Lets go hush mate . Backyard chemistry down under with ozbee



		encopo (Hive Bee) 10-15-01 21:35 No 224915				Re: A route to P2P
						An easier way to make benzal chloride is shown in the patent U.S. Pat.#1,280,612. Check out this excerpt from a recent post of mine in serious chemistry: "I've been looking around for a nice way to get some benzaldehyde to use in this. looking at the "phenylacetones.htm" file I found a patent reference for the production of benzyl chloride by the chlorination of toluene (it's the same thing as toluene with 1 xtra Cl on the carbon outcrop). The process bubbled Cl2 through Toluene, but it also said that using "bleaching powder" at high temperature with an acid provides nascent chlorine. However, the guy who wrote this has a bitch about side products. Now here is the NICE bit: "I have discovered, however...., by heating to a high temperature an anhydrous mixture of toluene and bleaching powder, with thorough commingling, and without the use of any acid, the chlorination of the toluene is effected without any of the disadvantages incident to the processes above referred to. In the absence of any added water the chlorin from the bleaching powder seems to go directly to produce benzyl chlorid in the side chain without attacking the nucleus, even though the process is carried on in the presence of iron, as in an iron vessel" Hmm. That looks nice. The reaction is pretty much: Heat toluene to 90'C. Slowly add equal amount (weight) of Ca(OCl)2 (pool shock), and raise temperature to 100'-105'C, leaving it there 1 hour or until reaction complete. Settle. Decant of oil. This oil contains 30-35% benzyl chloride and 65-70% toluene. However, We don't want benzyl chloride, do we? We want BENZAL chloride. The patent goes on to describe that if sufficient amount of Ca(OCl)2 is added, the toluene is completely converted to Benzal Chloride and Benzo Trichloride. Upon boiling in alkaline water, we get Benzaldehyde and Benzoic acid. Voila. Hope this will be a good addition to the home-brew-E method, as many bees don't have that much benzaldehyde lying around." I assume that what you're after is BENZAL chloride, but similiarly benzyl chloride and benzo trichloride could be prepared as above. Just be careful that you're reading BENZAL, not benzyl. As to the info that OZBEE seems to have dug up, I would be very interested in assisting in the exploration of this field, plus the "otc-ination". PM me oz for discussion. Don't mind me. I'm mentally ill.

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