HRID1667858

反应详情

EQUATION

反应方程式

HRID 1667858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 3-methoxy-1-methyl-1H-pyrazole-5-carboxylate (2.01 g, 11.8 mmol) in methanol (15 mL) was added 8N aqueous sodium hydroxide solution (3.00 mL), and the mixture was stirred at room temperature for 18 hr. 6N Hydrochloric acid (4.00 mL) was added to the mixture, and the mixture was concentrated under reduced pressure. Water was added to the residue, and the precipitate was collected by filtration, washed with water and air-dried. The precipitate was suspended in diisopropyl ether, and the mixture was stirred at 80° C. for 15 min. After allowing to cool to room temperature, the precipitate was collected by filtration, washed with diisopropyl ether, and dried under reduced pressure to give the title compound (746 mg, yield 40%) as a white solid.

WORKUP

后处理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. filtrationthe precipitate was collected by filtration
  4. washwashed with water
  5. customair-dried
  6. stirringthe mixture was stirred at 80° C. for 15 min
  7. temperatureto cool to room temperature
  8. filtrationthe precipitate was collected by filtration
  9. washwashed with diisopropyl ether
  10. customdried under reduced pressure