HRID570528

反应详情

EQUATION

反应方程式

HRID 570528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 mg (0.70 mmol) of 1-(2-fluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidamide were admixed with 3 ml of tert-butanol, 146 mg (0.70 mmol) of methyl 3,3-dicyano-2,2-dimethylpropanoate dissolved in 1.5 ml of tert-butanol and 94 mg (0.84 mmol) of potassium tert-butoxide, and the mixture was heated under reflux for 48 h. Water was added and the precipitate was filtered off. The filtrate was extracted with dichloromethane, and the organic phase was dried over sodium sulphate and concentrated on a rotary evaporator. The residue was stirred with water/ethanol. The solid was filtered off and dried under high vacuum. 102 mg (34% of theory) of the target compound were obtained.

WORKUP

后处理

  1. temperatureunder reflux for 48 h
  2. filtrationthe precipitate was filtered off
  3. extractionThe filtrate was extracted with dichloromethane
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. concentrationconcentrated on a rotary evaporator
  6. filtrationThe solid was filtered off
  7. customdried under high vacuum
  8. custom102 mg (34% of theory) of the target compound were obtained