HRID1691432

反应详情

EQUATION

反应方程式

HRID 1691432 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 6-[(4-tert-butylphenyl)sulfonyl]-2-(trifluoromethyl)-6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine-8-carbonitrile (0.60 g, 1.23 mmol, intermediate 54) in ethanol (6 mL) at rt was added hydroxylamine (0.24 mL of a 50% aqueous solution), and potassium carbonate (0.02 mL of a 0.8 M aqueous solution). After stirring at rt for 45 min, the reaction mixture was heated at 105° C. for 65 min in a microwave reactor. After cooling to rt, the precipitate was collected by filtration to provide the title compound. LC/MS: m/e 520.2 (M+H)+.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated at 105° C. for 65 min in a microwave reactor
  2. temperatureAfter cooling to rt
  3. filtrationthe precipitate was collected by filtration