HRID2371708

反应详情

EQUATION

反应方程式

HRID 2371708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 3.61 g of 4-(dibenz[b,e]oxepin-11(6H)-ylidene)piperidine, 2.6 g of ethyl 3-bromopropionate, 1.8 g of potassium carbonate and 25 ml of N,N-dimethylformamide was stirred at 80° C. for 2 hrs. After cooling, water was added to the reaction mixture and extracted with ether. The ether layer was washed with water and extracted with hydrochloric acid. The aqueous layer was made alkaline with potassium carbonate and extracted with ether. The ether layer was washed with water, dried and concentrated to give 4.2 g of yellowish brown liquid, which was purified by column chromatography on silica gel (eluent: chloroform) to give 3.9 g of pale yellow liquid.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washThe ether layer was washed with water
  4. extractionextracted with hydrochloric acid
  5. extractionextracted with ether
  6. washThe ether layer was washed with water
  7. customdried
  8. concentrationconcentrated