HRID2227470

反应详情

EQUATION

反应方程式

HRID 2227470 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution in dichloromethane (10 ml) of the compound (239 mg) obtained in Example 1b, triphenyl phosphine (345 mg) and carbon tetrabromide (436 mg) were sequentially added dropwise under cooling with ice. The reaction mixture was stirred for 2 hours under cooling with ice and then concentrated at reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:9) to give the titled compound (yield,47%).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. temperatureunder cooling with ice
  3. concentrationconcentrated at reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent; ethyl acetate:n-hexane=1:9)