HRID456643

反应详情

EQUATION

反应方程式

HRID 456643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-(1H-pyrazolo[3,4-b]pyridin-3-yl)-1H-pyrrole-3-carboxylic acid (100 mg, 0.43 mmol) (from Example 11) and thionyl chloride (0.2M in DCM, 10 mL) was heated to reflux for 2 hours. The reaction was concentrated, the residue was dissolved in DCM, to it was added glycinamide hydrochloride (242 mg, 2.19 mmol), followed by TEA. The mixture was then stirred at room temperature until the reaction was completed by TLC. The reaction was diluted with water and extracted with DCM. The combined DCM was concentrated and purified on a silica gel column to give the titled compound.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. concentrationThe reaction was concentrated
  4. dissolutionthe residue was dissolved in DCM, to it
  5. extractionextracted with DCM
  6. concentrationThe combined DCM was concentrated
  7. custompurified on a silica gel column