HRID1951073
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of rac-[(3S,4R)-1-(4-methanesulfonyl-piperazine-1-carbonyl)-4-phenyl-pyrrolidin-3-yl]-methyl-carbamic acid tert-butyl ester (0.86 g, 1.61 mmol) in CH2Cl2 (12 ml) was added TFA (3 ml) at RT. Stirring was continued over night. The reaction mixture was then concentrated under vacuo, the crude dissolved in CH2Cl2, washed with aq.NaHCO3 and the organic phase dried over Na2SO4. Purification by flash chromatography (SiO2, CH2Cl2/MeOH 95:5) yielded 0.68 g (98%) of the title compound as a white solid. ES-MS m/e: 401.3 (M+H+).
WORKUP
后处理
- waitwas continued over night
- concentrationThe reaction mixture was then concentrated under vacuo
- dissolutionthe crude dissolved in CH2Cl2
- washwashed with aq
- dry with materialNaHCO3 and the organic phase dried over Na2SO4
- customPurification by flash chromatography (SiO2, CH2Cl2/MeOH 95:5)