HRID54944

反应详情

EQUATION

反应方程式

HRID 54944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of sodium (28 mg), ethyl acetate (0.12 ml) and ethyl formate (0.10 ml) in dry toluene (0.5 ml) was stirred at ambient temperature for 14 hours under nitrogen. To the mixture was added 5-amino-4-(4-fluorophenyl)-3-(pyridin-4-yl)pyrazole (150 mg) in dry ethanol (1.5 ml) and the mixture was refluxed for 7 hours. The reaction mixture was cooled and the separated solid was collected and dried. The solid was dissolved in water (15 ml) and the solution was washed with ether. The aqueous solution was neutralized with diluted hydrochloric acid. The separated solid was collected, washed with water and dried to give 4,5-dihydro-3-(4-fluorophenyl)-5-oxo-2-(pyridin-4-yl)pyrazolo[1,5-a]pyrimidine (62 mg).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 7 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe separated solid was collected
  4. customdried
  5. dissolutionThe solid was dissolved in water (15 ml)
  6. washthe solution was washed with ether
  7. customThe separated solid was collected
  8. washwashed with water
  9. customdried