HRID1987567

反应详情

EQUATION

反应方程式

HRID 1987567 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

4-Chlorophenyl sulphonyl chloride (211 mg, 1.00 mmol) was added to a solution of (2S)-2-amino-5,5,5-trifluoro-3-(2,2,2-trifluoroethyl)-pentanoic acid methyl ester (267 mg, 1.00 mmol) and pyridine (0.45 mL, 3.00 mmol) in CH2Cl2 (5 mL) and the reaction was subsequently stirred for 18 h at 25° C. The solvent was removed in vacuo and the residue was dissolved in EtOAc (20 mL). This solution was washed with 1M HCl (2×10 mL) and brine (10 mL), dried over Na2SO4 and evaporated to afford a crude oil which was purified by flash chromatography eluting with 20:80 EtOAc:hexanes to provide the title compound (380 mg) as an oil in 86% yield. Mass Spectrum (−ESI): 446.0 [M−H]−.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in EtOAc (20 mL)
  3. washThis solution was washed with 1M HCl (2×10 mL) and brine (10 mL)
  4. dry with materialdried over Na2SO4
  5. customevaporated
  6. customto afford a crude oil which
  7. customwas purified by flash chromatography
  8. washeluting with 20:80 EtOAc