HRID2374208
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 5.9 g (30.55 mmol) of ethyl 3-(pyridin-4-yl)-3-oxopropionate, 5.0 g (30.55 mmol) of 5,5-dimethyl-1,4,5,6-tetrahydro-2-pyrimidinamine monohydrochloride (prepared by analogy to the method described in U.S. Pat. No. 4,262,122) and 6.33 g (45.82 mmol) of potassium carbonate in 60 ml of ethanol was heated at reflux temperature during 12 h. The cooled suspension was filtered and the solvent removed by evaporation. The residue obtained was dissolved in dichloromethane and washed with water. The organic phase was dried and evaporated to give 6.30 g (80%) of product as a beige solid. Mp.: 152-154° C.
WORKUP
后处理
- customprepared by analogy to the method
- temperatureat reflux temperature during 12 h
- filtrationThe cooled suspension was filtered
- customthe solvent removed by evaporation
- customThe residue obtained
- washwashed with water
- customThe organic phase was dried
- customevaporated