HRID2172676

反应详情

EQUATION

反应方程式

HRID 2172676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 3-bromo-4-methyl-N-(4-(2-(pyrrolidin-1-yl)ethyl)phenyl)benzamide (59 mg, 0.13 mmol) and 4-(3-(trifluoromethyl)phenyl)pyrimidin-2-amine (31 mg, 0.13 mmol), KOBut (22 mg, 0.2 mmol), Pd2(dba)3 (4.6 mg, 0.005 mmol) and Xantphos (4.6 mg, 0.008 mmol) in a microwave reaction vessel was suspended in 1 mL of THF. The reaction mixture was heated in a microwave at 150° C. for 90 min. After cooling, the mixture was diluted with DMF, and then filtered with a 0.45 μm microfilter. The obtained filtrate was separated by a semi-preparative HPLC. Collected product fraction was lyophilized to give pure product as a while powder. MS (ESI+) m/z 546.1 [M+H]+.

WORKUP

后处理

  1. customin a microwave reaction vessel
  2. temperatureAfter cooling
  3. filtrationfiltered with a 0.45 μm microfilter
  4. customThe obtained filtrate was separated by a semi-preparative HPLC
  5. customto give pure product as a while powder