HRID2213073

反应详情

EQUATION

反应方程式

HRID 2213073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Methyl-4-piperidinecarbonyl chloride hydrochloride (400 mg, 2.02 mmol) was added to a solution of 5-(2,3-difluorophenyl)-1H-pyrazolo[3,4-c]pyridin-3-ylamine (100 mg, 0.41 mmol) in pyridine (4.5 mL). The reaction mixture was stirred at reflux for 48 hours, allowed to cool and concentrated. Purification by column chromatography using 20% v/v of a 2M methanolic ammonia solution in chloroform as eluent, and subsequent treatment of the product with 1M hydrogen chloride in ether afforded the title compound as a solid.

WORKUP

后处理

  1. temperatureat reflux for 48 hours
  2. temperatureto cool
  3. concentrationconcentrated
  4. customPurification by column chromatography