HRID2374208

反应详情

EQUATION

反应方程式

HRID 2374208 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customprepared by analogy to the method
  2. temperatureat reflux temperature during 12 h
  3. filtrationThe cooled suspension was filtered
  4. customthe solvent removed by evaporation
  5. customThe residue obtained
  6. washwashed with water
  7. customThe organic phase was dried
  8. customevaporated