HRID1529164

反应详情

EQUATION

反应方程式

HRID 1529164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30 ml of tert-butanol, 1.068 g (6.429 mmol) of methyl 3,3-dicyano-2,2-dimethylpropanoate dissolved in 15 ml of tert-butanol and 901 mg (8.037 mmol) of potassium tert-butoxide were added to 1.400 g (5.358 mmol) of 1-(cyclopentylmethyl)-5-fluoro-1H-pyrazolo[3,4-b]pyridine-3-carboximidamide, and the mixture was heated under reflux for 24 h. The reaction mixture was concentrated on a rotary evaporator, triturated with 60 ml of water/ethanol (v/v=5:1), filtered off with suction and dried under high vacuum. This gave 1.296 g (57% of theory) of the target compound.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 24 h
  3. concentrationThe reaction mixture was concentrated on a rotary evaporator
  4. customtriturated with 60 ml of water/ethanol (v/v=5:1)
  5. filtrationfiltered off with suction
  6. customdried under high vacuum