HRID20204

反应详情

EQUATION

反应方程式

HRID 20204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 3.1 gr (8.1 mmol) of 5-(1H-Indole-3-carbonyloxy)-10-oxo-8-aza-tricyclo[5.3.1.03,8]undecane-9-carboxylic acid methyl ester and LiCl (0.69 gr, 16.23 mmol) in dimethylformamide (90 mL) is heated to 140° C. Once 4 hours have elapsed, and after checking by thin-layer chromatography (AcOEt/MeOH 9:1) that the reaction has been completed, the mixture is left to cool. Volatile substances are evaporated at low pressure and the residue is dissolved in dichloromethane (150 mL). This is washed with a saturated aqueous solution of NaCl (70 mL), and the organic phase is dried over magnesium sulphate and evaporated, to provide crude 1H-Indole-3-carboxylic acid 10-oxo-8-aza-tricyclo[5.3.1.03,8]undec-5-yl ester as a solid (2.18 gr, 83%).

WORKUP

后处理

  1. customOnce 4 hours
  2. waitthe mixture is left
  3. temperatureto cool
  4. customVolatile substances are evaporated at low pressure
  5. dissolutionthe residue is dissolved in dichloromethane (150 mL)
  6. washThis is washed with a saturated aqueous solution of NaCl (70 mL)
  7. dry with materialthe organic phase is dried over magnesium sulphate
  8. customevaporated