HRID3202

反应详情

EQUATION

反应方程式

HRID 3202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
175 °C

PROCEDURE

实验过程

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (4.10 mmol) of 2-methoxyaniline was heated, with stirring, in a 175° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ether (2 mL) was added. The crystals that developed were filtered and washed with 1 mL of ether; wt 0.070 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform. Recrystallization from ether gave pure product; wt 0.029 g; mp 200°-201° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureThe resulting solution was heated for 5 minutes
  3. temperaturecooled to room temperature
  4. filtrationThe crystals that developed were filtered
  5. washwashed with 1 mL of ether
  6. customThe solid was purified
  7. customto remove dark colors by silica gel chromatography
  8. washeluting with chloroform
  9. customRecrystallization from ether
  10. customgave pure product