HRID1241458

反应详情

EQUATION

反应方程式

HRID 1241458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-Chloro-2-[1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]-4,5-pyrimidinediamine (74 mg, 0.20 mmol) from example V was dissolved in MeOH (4 ml), and Pd/C (10%, 20 mg) and ammonium formate (126 mg, 2.00 mmol, 10 equivalents) were added. The mixture was heated under reflux for 2 days and then allowed to cool to room temperature before the catalyst was filtered off. Purification took place by preparative HPLC (column: Cromsil 120 ODS, C-18, 10 μm, 250×30 mm, flow rate 50 ml/min, room temperature, gradient: water acetonitrile at 0 min: 90:10, at 28 min 5:95) afforded the desired product.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 days
  3. filtrationwas filtered off
  4. customPurification
  5. customby preparative HPLC (column: Cromsil 120 ODS, C-18, 10 μm, 250×30 mm, flow rate 50 ml/min, room temperature, gradient: water acetonitrile at 0 min: 90:10, at 28 min 5:95)