HRID2367223
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 phenylmethyl(2S)-2-(hydroxymethyl)-1-pyrrolidinecarboxylate (0.78 g, 3.32 mmol) in CH2Cl2 (10 mL) was added Et3N (0.92 mL, 6.63 mmol) followed by TsCl (0.664 g, 3.48 mmol) and the reaction mixture was stirred overnight at room temperature. The mixture was poured onto water and diethyl ether (Et2O). The aqueous layer was separated and the organic layer was washed with saturated aqueous NaHCO3 followed by brine, dried (MgSO4), filtered and concentrated. Flash chromatography on SiO2 (gradient: 100% hexanes to 20% EtOAc/hexanes) afforded the title compound (0.85 g, 66%) as a colorless oil. LC-MS (ES) m/z=390 [M+H]+.
WORKUP
后处理
- customThe aqueous layer was separated
- washthe organic layer was washed with saturated aqueous NaHCO3
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated