HRID37932

反应详情

EQUATION

反应方程式

HRID 37932 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 ethyl 1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carboxylate (0.51 g, 2 mmol) in toluene (20 mL) was added Lawesson's reagent (1.45 g, 3.6 mmol). The resulting suspension was heated to reflux under nitrogen for 24 hours. Solvent was evaporated to give the crude product, which was purified by column chromatography on silica gel eluting with MeOH-DCM (1:19) to give 1,2,3,6-tetrahydroazepino[4,5-b]indole-5-carbothioic acid O-ethyl ester (27 mg); MS (ES): 273 (MH+).

WORKUP

后处理

  1. temperatureThe resulting suspension was heated
  2. temperatureto reflux under nitrogen for 24 hours
  3. customSolvent was evaporated
  4. customto give the crude product, which
  5. customwas purified by column chromatography on silica gel eluting with MeOH-DCM (1:19)