Proclival,Houde,France,1970
Buphenine is the starting material. See under the alternative name "Nylidrin"
in this publication for synthesis.
24 grams of buphenine hydrochloride are suspended in a mixture of 440 ml of
34% ammonia (specific gravity = 0.89) and 315 ml of water. 41 grams of
iodine dissolved in 1,080 ml of 96% alcohol are added little by little, with
good stirring. During this addition, effected in about 30 min, buphenine
hydrochloride dissolves fairly rapidly, and then the diiodobuphenine
precipitates out as a crystalline powder. Stirring is continued for a further
hour. The precipitate is suction filtered, and then washed with water, with
alcohol and with ether and is finally dried in vacuo in the exsiccator in the
presence of phosphoric anhydride. Thus, about 23 grams of diiodobuphenine
solvated with 1 mol of ethanol are obtained in the form of a microcrystalline
white powder. MP (slow) = 185°C (dec.). MP (inst.): 212°C.
