反应详情

温度

80 °C

30.83 g (80 mmol) of N-{4-[2-amino-3,5-dicyano-6-(phenylsulphanyl)-4-pyridinyl]-phenyl}-acetamide are dissolved in 120 ml of DMF under argon, after which 9.36 g (120 mmol) of sodium sulphide are added and the mixture is stirred at 80° C. for 2 hours. A solution of 20 ml of 1N aqueous HCl in 44 ml of water is then added dropwise at from 40 to 65° C., after which the crystals which have formed during this procedure are filtered off with suction and washed with water. The precipitate is suspended in 200 ml of methanol and stirred under reflux for 5 minutes. After cooling down to room temperature, the precipitate is filtered off with suction, washed with methanol and diethyl ether and dried in vacuo.

1. customafter which the crystals which have formed during this procedure
2. filtrationare filtered off with suction
3. washwashed with water
4. stirringstirred
5. temperatureunder reflux for 5 minutes
6. temperatureAfter cooling down to room temperature
7. filtrationthe precipitate is filtered off with suction
8. washwashed with methanol and diethyl ether
9. customdried in vacuo