HRID1858193
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
A mixture of 4 g (17.2 mmol) of ethyl 4-chloro-2-methylthiopyrimidine-5-carboxylate and 5 g (54 mmol) of aniline in 40 ml of dioxan was stirred at room temperature for 24 hours. The mixture was then evaporated and 100 ml of ethyl acetate and 50 ml of 2M aqueous hydrochloric acid were added to the residue. The phases were separated and the organic phase was washed with 50 ml of aqueous hydrochloric acid, dried over magnesium sulfate, filtered and evaporated. The resulting solid was purified by crystallisation from aqueous ethanol to give 3.5 g (64%) of ethyl 4-phenylamino-2-methylthiopyrimidine-5-carboxylate as a white solid.
WORKUP
后处理
- customThe mixture was then evaporated
- addition100 ml of ethyl acetate and 50 ml of 2M aqueous hydrochloric acid were added to the residue
- customThe phases were separated
- washthe organic phase was washed with 50 ml of aqueous hydrochloric acid
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated
- customThe resulting solid was purified by crystallisation from aqueous ethanol