HRID1951068

反应详情

EQUATION

反应方程式

HRID 1951068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 (640 mg, 1.38 mmol) in CH2Cl2 (10 ml) was added TFA (2 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 0.49 g (98%) of the title compound as a white solid. ES-MS m/e: 367.1 (M+H+).

WORKUP

后处理

  1. waitwas continued over night
  2. concentrationThe reaction mixture was then concentrated under vacuo
  3. dissolutionthe crude dissolved in CH2Cl2
  4. washwashed with aq. NaHCO3
  5. dry with materialthe organic phase dried over Na2SO4
  6. customPurification by flash chromatography (SiO2, CH2Cl2/MeOH 95:5)