HRID1372586
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
DIAD (4.13 ml, 21.0 mmol) was added to a solution of methyl (2S,4S)-1-tert-butoxycarbonyl-4-hydroxy-2-pyrrolidinylcarboxylate (4.69 g, 19.1 mmol), phenol (1.98 g, 21.0 mmol) and triphenylphosphine (5.51 g, 21.0 mmol) in THF (80 ml) under stirring at room temperature in a nitrogen gas stream. The reaction mixture was stirred overnight at room temperature. The residue obtained by concentrating the reaction mixture under reduced pressure was purified by chromatography on a silica gel column (silica gel: 700 g), whereby from chloroform/ethyl acetate (10/1) eluate fractions, the title compound (5.31 mg, 86%) was obtained as a colorless oil.
WORKUP
后处理
- stirringThe reaction mixture was stirred overnight at room temperature
- customThe residue obtained
- concentrationby concentrating the reaction mixture under reduced pressure
- customwas purified by chromatography on a silica gel column (silica gel: 700 g), whereby from chloroform/ethyl acetate (10/1) eluate fractions