HRID979978

反应详情

EQUATION

反应方程式

HRID 979978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (60 mg, 2.5 mmoles) was added to ethanethiol (124 mg, 2 mmoles) in dry DMF (2 ml) under argon. 7-Methoxy-1,4-diaza-10H-phenothiazine (462 mg, 2 mmoles) was then added and the reaction mixture was refluxed for 3 hours. The mixture was poured into 0.5N HCl (50 ml). The solid was collected, washed with methanol and air-dried to yield starting material. Extraction of the filtrate with ethyl acetate gave 100 mg of a mixture that was chromatographed on silica gel, eluting with 40% ethyl acetate in hexane to yield 25 mg of the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 3 hours
  2. customThe solid was collected
  3. washwashed with methanol
  4. customair-dried
  5. customto yield
  6. extractionExtraction of the filtrate with ethyl acetate