4-(4-chlorophenyl)-4-oxobutanenitrile

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: HCl and H2S gas are bubbled through a solution of the above nitrile (7.70 g, 40.0 mmol) in 100 ml of methanol at 10°-20° for 7 hours. The suspension is then stirred at RT overnight. It is dried, filtered, washed with ether and dried with suction under an N2 atmosphere to give 2-amino-5-(4-chlorophenyl)thiophene hydrochloric acid salt, a slightly purplish powder. It is dried filtered washed with ether dried with suction under an N2 atmosphere

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a mixture of freshly ground sodium cyanide (0.75 g, 15.0 mmol) in dimethylformamide (DMF) is added, over 30 min., 4-chlorobenzaldehyde (21.0 g, 150.0 mmol) in DMF. 30 Minutes after the addition is completed, acrylonitrile (5.96 g, 7.4 ml, 112.5 mmol) is added over a period of 1 hour. The mixture is stirred at RT for 3 hours, after which acetic acid (0.99 g, 0.94 ml, 16.5 mmol) is added. After 5 min., the reaction mixture is poured into water and extracted with chloroform. The combined chloroform layers are washed with water and with brine, dried and stripped of solvent. The residue is recrystallized and filtered to give 4-(4-chlorophenyl)-4-oxobutyronitrile. is added, over 30 min. 30 Minutes after the addition After 5 min. extracted with chloroform The combined chloroform layers are washed with water and with brine dried The residue is recrystallized filtered