HRID1093447

反应详情

EQUATION

反应方程式

HRID 1093447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A suspension of Compound 67-1 (3.08 g) and chlorotris(triphenylphosphine)rhodium(I) (3.00 g) in toluene (70 ml) was stirred under a hydrogen atmosphere at 65° C. for 11 hr. The reaction mixture was concentrated, diisopropyl ether was added and the mixture was filtered through celite. The filtrate was concentrated and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-75:25) to give the object product (2.49 g) as a brown oil.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiisopropyl ether was added
  3. filtrationthe mixture was filtered through celite
  4. concentrationThe filtrate was concentrated
  5. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=99:1-75:25)