HRID1349943

反应详情

EQUATION

反应方程式

HRID 1349943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of tert-butyl 4-(5-bromo-2-methoxy-3-nitrobenzylidene)piperidine-1-carboxylate (2.5 g, 5.9 mmol) and lithium chloride (1 g) in anhydrous N,N-dimethylformamide was stirred at 120° C. for 4 h. It was allowed to cool to room temperature and evaporated in vacuo. The residue was treated with water (50 mL) and extracted with diethyl ether (2×100 mL). The combined organic layers was washed with water (50 mL) and dried (Na2SO4). Evaporation of solvent gave the title compound as a crude oil (2.1 g).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. customevaporated in vacuo
  3. additionThe residue was treated with water (50 mL)
  4. extractionextracted with diethyl ether (2×100 mL)
  5. washThe combined organic layers was washed with water (50 mL)
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of solvent