HRID1078964
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 4 hours
- customevaporated
- customAfter separation the organic phase
- washis washed 4 times with 10 ml of water each,
- customthen dried
- customevaporated
- customAfter recrystallizing the obtained product from hexane the title compound
- customis obtained in a yield of 2.51 g (91%), m.p.: 130°-131° C.