HRID1078964

反应详情

EQUATION

反应方程式

HRID 1078964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After adding 2.6 ml (17.23 mmoles) of 1,4-dioxa-8-azaspiro[4,5]decane to the solution of 2.0 g (6.89 mmoles) of 2-(4,4-ethylenedioxy-1-piperidinyl)-4,6-dichloropyrimidine in 40 ml of n-butanol, the reaction mixture is boiled under reflux for 4 hours, then evaporated. The evaporation residue is distributed between 50 ml of chloroform and 5 ml of 10% sodium hydroxide solution. After separation the organic phase is washed 4 times with 10 ml of water each, then dried and evaporated. After recrystallizing the obtained product from hexane the title compound is obtained in a yield of 2.51 g (91%), m.p.: 130°-131° C.

WORKUP

后处理

  1. temperatureunder reflux for 4 hours
  2. customevaporated
  3. customAfter separation the organic phase
  4. washis washed 4 times with 10 ml of water each,
  5. customthen dried
  6. customevaporated
  7. customAfter recrystallizing the obtained product from hexane the title compound
  8. customis obtained in a yield of 2.51 g (91%), m.p.: 130°-131° C.