HRID2268555

反应详情

EQUATION

反应方程式

HRID 2268555 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 (56 mg), p-methoxyphenol (78 mg), and triphenylphosphine (69 mg) in THF (1 ml) was added a solution of diethyl azodicarboxylate (45, 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 recrystallized from ethyl acetate-hexane to obtain the entitled compound (68 mg).

WORKUP

后处理

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