HRID1958322

反应详情

EQUATION

反应方程式

HRID 1958322 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Chlorocarbonyl-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (3.60 g, assumed purity 60%, 10 mmol) was added slowly to a cooled (0° C.) solution of 2-phenylimidazo[1,2-a]pyrimidin-7-amine (example 1, step 1, 2.52 g, 12 mmol) and triethylamine (2.02 g, 20 mmol) in dichloromethane (50 ml), and the suspension was stirred overnight at RT. The mixture was taken up in dichloromethane, and washed with water. The combined organic layers were dried (Na2SO4), filtered, and the solvent was evaporated under reduced pressure. The title compound (2.75 g, 71%) was isolated from the residue by column chromatography (silica gel, heptane:ethyl acetate=100:0-60:40). MS (m/e)=391.2 [M+H+].

WORKUP

后处理

  1. washwashed with water
  2. dry with materialThe combined organic layers were dried (Na2SO4)
  3. filtrationfiltered
  4. customthe solvent was evaporated under reduced pressure