反应详情

A solution of 1-(3-aminophenyl)-1,4-dihydroisoquinol-3-one (8.0 g) in dichloromethane (500 ml) and triethylamine (50 ml) was treated dropwise, at room temperature, with a solution of mesyl chloride (9.7 g) in dichloromethane (20 ml). After stirring for 3 h, the resulting precipitate (m.p. 251°-253° C.) was collected, washed with dichloromethane, water, and air dried. The product was stirred with a mixture of 10% aqueous sodium hydroxide (200 ml) and methanol (20 ml) at 50° C. for 1 h. The mixture was filtered and the filtrate was evaporated to one third volume in vacuo. It was acidified with dilute hydrochloric acid, and the resulting precipitate was collected and washed with water. Recrystallisation from methanol-ether afforded the title compound (3.55 g)

1. customthe resulting precipitate (m.p. 251°-253° C.) was collected
2. washwashed with dichloromethane, water, and air
3. customdried
4. stirringThe product was stirred with a mixture of 10% aqueous sodium hydroxide (200 ml) and methanol (20 ml) at 50° C. for 1 h
5. filtrationThe mixture was filtered
6. customthe filtrate was evaporated to one third volume in vacuo
7. customthe resulting precipitate was collected
8. washwashed with water
9. customRecrystallisation from methanol-ether