HRID1029637
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
A solution of (2S,4R)-4-(tert-butyldimethylsilyloxy)-1-(tert-butoxycarbonyl)-2-methoxymethylpyrrolidine (4.48 g) and tetrabutylammonium fluoride (1 Mol tetrahydrofuran solution, 13 ml) in tetrahydrofuran (45 ml) was stirred at 0° C. for eight hours. The reaction mixture was extracted with ethyl acetate, and the organic layer was separated, washed with brine, dried over magnesium sulfate. Evaporation of the solvent gave an oil, which was chromatographed on silica gel (300 ml) eluting with a mixture of hexane and ethyl acetate (1:2, V/V) to give (2S,4R)-1-(tert-butoxycarbonyl-4-hydroxy-2-methoxymethylpyrrolidine (2.82 g).
WORKUP
后处理
- extractionThe reaction mixture was extracted with ethyl acetate
- customthe organic layer was separated
- washwashed with brine
- dry with materialdried over magnesium sulfate
- customEvaporation of the solvent
- customgave an oil, which
- customwas chromatographed on silica gel (300 ml)
- washeluting with a mixture of hexane and ethyl acetate (1:2, V/V)