HRID2050509

反应详情

EQUATION

反应方程式

HRID 2050509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 10.0 g of 4,5-dihydro-7-(3-(trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide (prepared as described in Example 8) in 200 ml of dioxane at room temperature under nitrogen is added 20.0 g of 1,1'-carbonyldiimidazole. The mixture is then heated at reflux for 5 hours, and then is cooled and filtered. The filtrate is evaporated to dryness in vacuo and an excess of water is added to the residue. The white solid which forms is collected and is recrystallized from acetonitrile-ethanol to give 6.5 g of the desired product as a white solid, mp 260-262° C.

WORKUP

后处理

  1. temperatureThe mixture is then heated
  2. temperatureat reflux for 5 hours
  3. temperatureis cooled
  4. filtrationfiltered
  5. customThe filtrate is evaporated to dryness in vacuo
  6. additionan excess of water is added to the residue
  7. customThe white solid which forms is collected
  8. customis recrystallized from acetonitrile-ethanol