HRID2268554

反应详情

EQUATION

反应方程式

HRID 2268554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 7-(2-hydroxyethyl)-2,3-dimethoxy-4,5,6,7,8,9-hexahydro-1H-benzo[a]cycloheptene-1,4-dione (103 mg), p-cyanophenol (127 mg), triphenylphosphine (126 mg) in THF (2 ml) was added a solution of diethyl azodicarboxylate (90 mg) in THF (1 ml) at room temperature. The reaction mixture was stirred at room temperature for 2 hr and then concentrated in vacuo. The residue was purified by alumina column chromatography (ethyl acetate:hexane=1:4) and then with recrystallization from ethyl acetate-hexane to obtain the entitled compound (118 mg).

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified by alumina column chromatography (ethyl acetate:hexane=1:4)
  3. customwith recrystallization from ethyl acetate-hexane