HRID604856
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 0° C. suspension of LiBH4 (2.0 equiv) in THF (0.5 M) was slowly added TMSCl (4.0 equiv) by syringe. After stirring at room temperature for 30 minutes, (2S,3S)-1-(tert-butoxycarbonyl)-3-hydroxypyrrolidine-2-carboxylic acid (1.0 equiv) was then added, and the resulting mixture was stirred at room temperature overnight. The reaction was quenched by the careful addition of sat'd. aq. NaHCO3, and the mixture was diluted with EtOAc, and the organic layer was washed twice with sat'd. aq. NaHCO3, once with brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. The title compound was isolated in 55% yield and used without further purification.
WORKUP
后处理
- stirringthe resulting mixture was stirred at room temperature overnight
- customThe reaction was quenched by the careful addition of sat'd
- additionaq. NaHCO3, and the mixture was diluted with EtOAc
- washthe organic layer was washed twice with sat'd
- dry with materialaq. NaHCO3, once with brine, dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo