HRID2268557
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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-cresol (118 mg) and triphenylphosphine (121 mg) in THF (2 ml) was added a solution of diethyl azodicarboxylate (87 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=1:10) and then with recrystallization from duisopropylether-hexane to obtain the entitled compound (80 mg).
WORKUP
后处理
- concentrationconcentrated in vacuo
- customThe residue was purified by alumina column chromatography (ethyl acetate:hexane=1:10)
- customwith recrystallization from duisopropylether-hexane