HRID1078944

反应详情

EQUATION

反应方程式

HRID 1078944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After dissolving 5.0 g of 2,4-dichloro-6-(1,1-dimethylethylamino)pyrimidine in 25 ml of isopropanol and adding 5 ml of 1-amino-2,2-dimethylpropane, the reaction mixture is boiled under reflux for 20 hours. Subsequently, the reaction mixture is evaporated and the residue is distributed between 80 ml of chloroform and 15 ml of 10% sodium hydroxide solution. After separation the organic phase is washed 4 times with 20 ml of water each, then dried and evaporated. The evaporation residue is purified by chromatography on a silica gel column by using a 9:1 mixture of hexane/ethyl acetate as eluent. After recrystallizing the eluted product from hexane, the title product is obtained in a yield of 4.05 g (65.9%), m.p.: 115°-119° C.

WORKUP

后处理

  1. temperatureunder reflux for 20 hours
  2. customSubsequently, the reaction mixture is evaporated
  3. customAfter separation the organic phase
  4. washis washed 4 times with 20 ml of water each,
  5. customthen dried
  6. customevaporated
  7. customThe evaporation residue is purified by chromatography on a silica gel column
  8. additiona 9:1 mixture of hexane/ethyl acetate as eluent
  9. customAfter recrystallizing the eluted product from hexane