HRID1409114

反应详情

EQUATION

反应方程式

HRID 1409114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (S)-2-amino-N-(2,2,2-trifluoroethyl)propanamide (FF) (1 g, 3.35 mol, 1 equiv.) in iso-propanol (10 mL), Huning's base (1.5 mL) was added, followed by 2,4-dichloropyrimidine (JJ). The resulting mixture was refluxed for 18 h. The reaction mixture was then diluted in ethyl acetate, washed with aqueous HCl 0.5 M and water, and dried over anhydrous Na2SO4. The crude oil was then purified by flash chromatography on silica gel, eluting with hexanes/ethyl acetate mixtures (100:0 to 0:100). The title compound HH was isolated as a white solid (600 mg, 63%).

WORKUP

后处理

  1. temperatureThe resulting mixture was refluxed for 18 h
  2. washwashed with aqueous HCl 0.5 M and water
  3. dry with materialdried over anhydrous Na2SO4
  4. customThe crude oil was then purified by flash chromatography on silica gel
  5. washeluting with hexanes/ethyl acetate mixtures (100:0 to 0:100)