反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of the methyl 10-(4-cyclohexylbenzoyl)-3-[(4-methyl-1-piperazinyl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-8-carboxylate of Example 1, Step D (1.1 g, 1.93 mmol) in ethanol (10 mL) was added 2.5 N sodium hydroxide (1.5 equiv.) and the reaction mixture was stirred overnight at room temperature. The solution was neutralized by the addition of one equivalent of 2 N hydrochloric acid and the solvent was removed in vacuo. The residue was extracted with dichloromethane, filtered and the solvent removed in vacuo. The residue was then chromatographed on silica gel eluting with 10% methanol in dichloromethane to provide the title product as a white crystalline solid, m.p. 195–210° C.
WORKUP
后处理
- customthe solvent was removed in vacuo
- extractionThe residue was extracted with dichloromethane
- filtrationfiltered
- customthe solvent removed in vacuo
- customThe residue was then chromatographed on silica gel eluting with 10% methanol in dichloromethane