反应详情

A solution of 2N sodium hydroxide (6 mL, 1.2 mmol) was added in three portions over two hr to a solution of 6-cyano-11-cyclopropyl-4-methyl-11H-dipyrido[3,2-b:2',3'-e][1,4]diazepine (0.30 g, 1.1 mmol) in methanol (50 mL) at room temperature. The mixture was stirred overnight, and then concentrated in vacuo. The residue was dissolved in ethyl acetate (150 mL) and washed succesively with water and brine. After drying (MgSO4), the solution was concentrated and crystallized from acetonitrile to give 0.20 g (65%) of the title compound. A second recrystallization from methanol provided pure product, m.p. 191°-192° C.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate (150 mL)
3. washwashed succesively with water and brine
4. dry with materialAfter drying (MgSO4)
5. concentrationthe solution was concentrated
6. customcrystallized from acetonitrile