HRID1251939

反应详情

EQUATION

反应方程式

HRID 1251939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

39.5 g (0.2 mol) of 5-methyl-2,4,6-trichloropyrimidine are dissolved in 250 ml of dimethoxyethane, and ammonia gas is then introduced at room temperature until the solution is saturated. A white suspension is formed, which is stirred for 12 hours at room temperature; it is subsequently concentrated in a rotary evaporator, and 200 ml of water are added to the residue. The formed suspension is filtered and the precipitate is dried. The mother liquor is concentrated to half the volume, filtered, and the precipitate is dried. There are thus obtained 26.4 g of crude product, which is recrystallised from acetonitrile/water (5:1); m.p. 193°-194° C. (yield=75% of theory).

WORKUP

后处理

  1. customA white suspension is formed
  2. concentrationit is subsequently concentrated in a rotary evaporator, and 200 ml of water
  3. additionare added to the residue
  4. filtrationThe formed suspension is filtered
  5. customthe precipitate is dried
  6. concentrationThe mother liquor is concentrated to half the volume
  7. filtrationfiltered
  8. customthe precipitate is dried
  9. customis recrystallised from acetonitrile/water (5:1)