HRID1776430

反应详情

EQUATION

反应方程式

HRID 1776430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

50 mg of 4-amino-2-[1-(2-fluorobenzyl)-1H-indazol-3-yl]pyrimidin-5-ol (1-11-1, 0.149 mmol, 1. eq.) were dissolved in 3 ml of N,N-dimethylformamide. 103 mg of potassium carbonate (0.746 mmol, 5 eq.) and 32.8 mg of 4-bromopyridine-3-carbonitrile (0.179 mmol, 1.2 eq.) were added. The reaction mixture was stirred at 100° C. bath temperature for 18 hours. After cooling at room temperature the mixture was filtered off and washed with dichloromethane. The filtrate was concentrated in vacuo. The residue was purified by preparative HPLC and preparative TLC to yield 4.21 mg (0.01 mmol, 6.1%) of the analytically pure target compound.

WORKUP

后处理

  1. temperatureAfter cooling at room temperature the mixture
  2. filtrationwas filtered off
  3. washwashed with dichloromethane
  4. concentrationThe filtrate was concentrated in vacuo
  5. customThe residue was purified by preparative HPLC and preparative TLC
  6. customto yield 4.21 mg (0.01 mmol, 6.1%) of the analytically pure target compound