反应详情

温度

60 °C

A mixture of chloroacetonitrile (2.15 ml) and (4-piperidinyl)-methyl 8-amino-7-chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylate (11 g) in N,N-diethylethanamine (7 ml) and DMF (150 ml) was stirred at 60° C. until the reaction was complete. Then, the mixture was cooled. The solvent was evaporated. The residue was partitioned between DCM and water. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was crystallized from ACN and the precipitate was filtered off and dried (vacuum, 50° C.), yielding 6.6 g (53%) [1-(cyanomethyl)-4-piperidinyl]-methyl 8-amino-7-chloro-2,3-dihydro-1,4-benzodioxin-5-carboxylate (intermediate 14).

1. temperatureThen, the mixture was cooled
2. customThe solvent was evaporated
3. customThe residue was partitioned between DCM and water
4. customThe separated organic layer was dried
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe residue was crystallized from ACN
8. filtrationthe precipitate was filtered off
9. customdried (vacuum, 50° C.)