HRID1270179

反应详情

EQUATION

反应方程式

HRID 1270179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe solvent was removed in vacuo
  2. extractionThe residue was extracted with dichloromethane
  3. filtrationfiltered
  4. customthe solvent removed in vacuo
  5. customThe residue was then chromatographed on silica gel eluting with 10% methanol in dichloromethane