bwitiacumen
01-25-2005, 11:20 PM
In Uncle Fester's "Practical LSD Manufacture", in the bonus TMA-2 section, here's an electro-reduction I found:
“Now to do the electric reduction, four grams of the B-nitro asarone are dissolved in 150ml ethanol and 50ml of acetic acid. Then add 10ml concentrated hydrochloric acid. This is the catholyte. Both cathode and anode are made of lead. Obtain “lead Hull cell anodes” price – about $9 each. You like to play around with plating chrome, don’t ya know? These chunks of pure lead, about 2 inches square and about ¼ inch thick, can be beaten easily into thinner material. The actual size of the anode and cathode isn’t specified, but they should be of roughly equal surface area, and be as large as will fit into the beaker used as the reaction container. Make sure they can’t contact each other to make a short, as the current must flow through the solution, The cathode is cylinder-shaped, the metal about 1mm thick, with holes drilled in it to allow passage of current from the solution to the inner surface, and the flow of catholyte. The anode is a sheet of lead. The anolyte inside the dialysis tubing in contact with the anode is 20% by weight sulfuric acid diluted with water. The bottom of the dialysis tubing should be tied very tight to prevent leakage. The top should be looser to allow bubbles of O2 to escape.
The anode is connected to the DC+ pole of a transformer, and the cathode is connected to the DC- pole of the same transformer. A good amp meter should be put in line to measure current, as this is crucial to control. All this electric equipment can be had at *adio S**ck.
Chill the reaction mixture in ice, then with vigorous magnetic stirring, apply .07 amps per square centimeter of the cathode immersed in the solution. When measuring this area, measure cylinder surface on the outside and inside of the hollow cylinder cathode, and subtract out the hole’s area. When making contact with alligator clips to the anode and cathode, be sure that both present a clean metal surface, and dig them in well. Lack of current passage will result from not making a good contact on both poles. The meter reading will make this obvious.
Pass current until the initially yellow- or orange-colored solution clears. Then take the catholyte, and reduce its volume to about 20ml under a vacuum. Make the residue alkaline to +12 to litmus with NaOH solution, with good shaking to ensure conversion of the salt to the free base, then extract out the TMA-2 free base with ether or toluene. The ether or toluene solution should then be bubbled with dry HCl to yield crystals of TMA-2 hydrochloride. Dry under a vacuum, and store in a freezer. If they are colored or sort of gooey and sloppy, recrystallize by dissolving the HCl salt in the minimum amount of alcohol, then add 20+ volumes of ether with shaking. Then filter and dry under a vacuum.”
Reference: J. Pract. Chem, Vol. 138, Page 271 (1933)
Here's my idea; Instead of applying this to pseudonitrosites, why not use it to hydrogenate codeine to hydrocodone? Is there anyone here that's taken college organic chem. courses that can provide an educated guess?
“Now to do the electric reduction, four grams of the B-nitro asarone are dissolved in 150ml ethanol and 50ml of acetic acid. Then add 10ml concentrated hydrochloric acid. This is the catholyte. Both cathode and anode are made of lead. Obtain “lead Hull cell anodes” price – about $9 each. You like to play around with plating chrome, don’t ya know? These chunks of pure lead, about 2 inches square and about ¼ inch thick, can be beaten easily into thinner material. The actual size of the anode and cathode isn’t specified, but they should be of roughly equal surface area, and be as large as will fit into the beaker used as the reaction container. Make sure they can’t contact each other to make a short, as the current must flow through the solution, The cathode is cylinder-shaped, the metal about 1mm thick, with holes drilled in it to allow passage of current from the solution to the inner surface, and the flow of catholyte. The anode is a sheet of lead. The anolyte inside the dialysis tubing in contact with the anode is 20% by weight sulfuric acid diluted with water. The bottom of the dialysis tubing should be tied very tight to prevent leakage. The top should be looser to allow bubbles of O2 to escape.
The anode is connected to the DC+ pole of a transformer, and the cathode is connected to the DC- pole of the same transformer. A good amp meter should be put in line to measure current, as this is crucial to control. All this electric equipment can be had at *adio S**ck.
Chill the reaction mixture in ice, then with vigorous magnetic stirring, apply .07 amps per square centimeter of the cathode immersed in the solution. When measuring this area, measure cylinder surface on the outside and inside of the hollow cylinder cathode, and subtract out the hole’s area. When making contact with alligator clips to the anode and cathode, be sure that both present a clean metal surface, and dig them in well. Lack of current passage will result from not making a good contact on both poles. The meter reading will make this obvious.
Pass current until the initially yellow- or orange-colored solution clears. Then take the catholyte, and reduce its volume to about 20ml under a vacuum. Make the residue alkaline to +12 to litmus with NaOH solution, with good shaking to ensure conversion of the salt to the free base, then extract out the TMA-2 free base with ether or toluene. The ether or toluene solution should then be bubbled with dry HCl to yield crystals of TMA-2 hydrochloride. Dry under a vacuum, and store in a freezer. If they are colored or sort of gooey and sloppy, recrystallize by dissolving the HCl salt in the minimum amount of alcohol, then add 20+ volumes of ether with shaking. Then filter and dry under a vacuum.”
Reference: J. Pract. Chem, Vol. 138, Page 271 (1933)
Here's my idea; Instead of applying this to pseudonitrosites, why not use it to hydrogenate codeine to hydrocodone? Is there anyone here that's taken college organic chem. courses that can provide an educated guess?