HRID2085027

反应详情

EQUATION

反应方程式

HRID 2085027 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of (5S)-3,9,10,11-tetramethoxy-6,7-dihydro-5H-dibenzo[a,c]cyclohepten-5-ylamine [Collect. Czech. Chem. Commun. 1999, 64(2), 217-228] (0.263 g; 0.8 mmol), 4-nitrophenylchloroformate (0.177 g; 0.88 mmol) and triethylamine (0.123 ml; 0.88 mmol) in acetonitrile (5 ml) was stirred under argon atmosphere for 2 hours at ambient temperature; 4-(2-hydroxyethyl)morpholine (0.145 ml; 1.2 mmol) in solution in acetonitrile (2 ml) was then added to the above solution. The mixture was heated at 60° C. overnight. After evaporation to dryness, the residue was purified by flash chromatography, eluted with ethanol/dichloromethane (4/96) to give the title compound.

WORKUP

后处理

  1. customAfter evaporation to dryness
  2. customthe residue was purified by flash chromatography
  3. washeluted with ethanol/dichloromethane (4/96)