反应详情

温度

25 °C

To a stirred suspension of 60% sodium hydride (0.52 g) in dimethylformamide (20 ml) is added under ice-coolinga solution of ethanethiol (0.81 g) in dimethylformamide (5 ml). After the mixture is stirred at 25° C. for 0.5 hour, 4-amino-N-[(4-benzyl-2-morpholinyl)methyl]-5-chloro-2-methoxybenzamide (3.4 g) is added, and the mixture is stirred at 100° C. for 1 hour. After cooling, the reaction mixture is evaporated under reduced pressure. The residue is diluted with water, washed with chloroform, and neutralized with 10% hydrochloric acid. The precipiate is collected, washed with water, and recrystallized from isopropyl alcohol to give the monohydrate of the title compound (2.3 g), mp 153°-155° C.

1. stirringthe mixture is stirred at 100° C. for 1 hour
2. temperatureAfter cooling
3. customthe reaction mixture is evaporated under reduced pressure
4. additionThe residue is diluted with water
5. washwashed with chloroform
6. customThe precipiate is collected
7. washwashed with water
8. customrecrystallized from isopropyl alcohol