HRID53632

反应详情

EQUATION

反应方程式

HRID 53632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.321 g (1.0 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7-(8H)-one from Example 12 and 0.404 g (1.0 mmol) of Lawesson's Reagent in 10 mL of pyridine was heated at reflux with stirring for 24 hours. The solvent was evaporated under reduced pressure, and the residue was triturated with 20 mL of water, filtered, and the cake washed well with water. Purification was by silica gel chromatography to afford the desired compound identified as 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]-pyrimidin-7(8H)-thione.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was triturated with 20 mL of water
  5. filtrationfiltered
  6. washthe cake washed well with water
  7. customPurification