Need some one to make basic formula for coc starts by purchasing or making tropinine,
converting the tropinone into 2-carbomethoxytropinone (also known as
methyl-tropan-3-one-2-carboxylate), reducing this to ecgonine,
and changing that to cocaine.
Succindialdehyde. This can be purchased, too. 23.2 g of succinaldoxime
powder in 410 ml of 1 N sulfuric acid and add dropwise with stirring at
0* a solution of 27.6 g of sodium nitrite in 250 ml of water over
3 hours. After the addition, stir and let the mixture rise to room temp
for about 2 hours, taking care not to let outside air into the reaction.
Stir in 5 g of Ba carbonate and filter. Extract the filtrate with ether
and dry, evaporate in vacuo to get the succindialdehyde. This was t
aken from JOC, 22, 1390 (1957). To make succinaldoxime, see JOC, 21,
644 (1956).
Complete Synthesis of Succindialdehyde. JACS, 68, 1608 (1946). In a 2 liter
3 necked flask equipped with a stirrer, reflux condenser, and an addition
funnel, is mixed 1 liter of ethanol, 67 g of freshly distilled pyrrole, and
141 g of hydroxylamine hydrochloride. Heat to reflux until dissolved, add
106 g of anhydrous sodium carbonate in small portions as fast as reaction
will allow. Reflux for 24 hours and filter the mixture. Evaporate the
filtrate to dryness under vacuo. Take up the residue in the minimum amount
of boiling water, decolorize with carbon, filter and allow to recrystallize
in refrigerator. Filter to get product and concentrate to get additional
crop. Yield of succinaldoxime powder is a little over 40 g, mp is 171-172*.
5.8 g of the above powder is placed in a beaker of 250 ml capacity and
54 ml of 10% sulfuric acid is added. Cool to 0* and add in small portions
of 7 g of sodium nitrite (if you add the nitrite too fast, nitrogen dioxide
fumes will evolve). After the dioxime is completely dissolved, allow the
solution to warm to 20* and effervescence to go to completion. Neutralize
the yellow solution to litmus by adding small portions of barium carbonate.
Filter off the barium sulfate that precipitates. The filtrate is 90% pure
succindialdehyde and is not purified further for the reaction to create
tropinone. Do this procedure 3 more times to get the proper amount for the
next step, or multiply the amounts given by four and proceed as described
above.
Take the total amount of succinaldehyde (obtained from 4 of the above
syntheses combined) and without further treatment or purification (this had
better be 15.5 g of succindialdehyde) put into an Erlenmeyer flask of
4-5 liters capacity. Add 21.6 g of methylamine hydrochloride, 46.7 g of
acetonedicarboxylic acid, and enough water to make a total volume of 2
liters. Adjust the pH to 8-10 by slowly adding a saturated solution of
disodium phosphate. The condensate of this reaction (allow to set for
about 6 days) is extracted with ether, the ethereal solution is dried
over sodium sulphate and distilled, the product coming over at 113* at
25 mm of pressure is collected. Upon cooling, 14 g of tropinone
crystallizes in the pure state.
2-Carbomethoxytropinone. A mixture of 1.35 g of sodium methoxide
(this is sodium in a minimum amount of methanol), 3.5 g of tropinone,
4 ml of dimethylcarbonate and 10 ml of toluene is refluxed for 30 min.
Cool to 0* and add 15 ml of water that contains 2.5 g of ammonium chloride.
Extract the solution after shaking with with four 50 ml portions of
chloroform, dry, evaporate the chloroform in vacuo. Dissolve the oil
residue in 100 ml of ether, wash twice with a mixture of 6 ml of
saturated potassium car