HRID570527

反应详情

EQUATION

反应方程式

HRID 570527 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under an argon atmosphere, 994 mg (purity 81%, approx. 3.01 mmol) of 1-(2-fluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carbonitrile were dissolved in 15 ml of absolute methanol. 209 mg (3.72 mmol) of sodium methoxide were added and the mixture was stirred at RT for 1 h. Subsequently, 31 mg (0.56 mmol) of sodium methoxide were added and the mixture was stirred at RT for 15 min. 871 mg (14.50 mmol) of acetic acid and 489 mg (4.46 mmol) of ammonium chloride were added and the mixture was stirred at 45° C. for 45 min. The reaction mixture was concentrated, the residue was stirred with 1N sodium hydroxide solution, and the precipitate was filtered off with suction and dried under high vacuum. 918 mg (purity 91%, 97% of theory) of the target compound were obtained.

WORKUP

后处理

  1. stirringthe mixture was stirred at RT for 15 min
  2. stirringthe mixture was stirred at 45° C. for 45 min
  3. concentrationThe reaction mixture was concentrated
  4. stirringthe residue was stirred with 1N sodium hydroxide solution
  5. filtrationthe precipitate was filtered off with suction
  6. customdried under high vacuum
  7. custom918 mg (purity 91%, 97% of theory) of the target compound were obtained