HRID1527350

反应详情

EQUATION

反应方程式

HRID 1527350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (2R,5S)-2-azidomethyl-5-(3-trifluoromethoxy-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid benzyl ester (460 mg, 0.99 mmol) and triphenylphosphine (312 mg, 1.19 mmol) in THF (4 mL) was stirred at RT overnight. After completion of the reaction, THF was removed and the crude reaction mixture was purified by preparative HPLC (Waters SunFire C18-ODB 5 μm, 19×50, 5-100% CH3CN/H2O in 17 min, 100% CH3CN for 3 min, CH3CN and H2O containing 0.1% TFA, flow: 20 mL/min) to give the title compound. MS: 438 [M+H]+; tR (HPLC conditions b): 3.8 min.

WORKUP

后处理

  1. customwas removed
  2. customthe crude reaction mixture
  3. customwas purified by preparative HPLC (Waters SunFire C18-ODB 5 μm, 19×50, 5-100% CH3CN/H2O in 17 min, 100% CH3CN for 3 min, CH3CN and H2O containing 0.1% TFA, flow: 20 mL/min)