HRID223136

反应详情

EQUATION

反应方程式

HRID 223136 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 5.8 g (0.02 mole) 5-chloro-4-hydroxy-6-methyl-2-trichloromethylpyrimidine and 2.0 g (0.02 mole) triethylamine in 100 ml diethyl ether was added 3.6 g (0.02 mole) trichloroacetyl chloride. After the exothermic reaction subsided, the reaction mixture was stirred an additional 10 minutes and filtered. The filtrate was concentrated in-vacuo and the residue recrystallized from ligroin to give 1.6 g starting material and 2.3 g product; m.p. 92° C. The corrected yield was 35%.

WORKUP

后处理

  1. customAfter the exothermic reaction
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in-vacuo
  4. customthe residue recrystallized from ligroin
  5. customto give 1.6 g