HRID878032

反应详情

EQUATION

反应方程式

HRID 878032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A solution of N-(4-bromo-pyridin-3-yl)-N-methyl-3,5-bis-trifluoromethyl-benzamide (example 25, intermediate a) (200 mg, 0.468 mmol), 3,6-dimethoxylpyridazine-4-boronic acid (129 mg, 0.702 mmol, CAS RN 1015480-87-1) and K2CO3 (194 mg, 1.404 mmol) in DMF (6 mL) in a sealed tube was degassed with argon for 30 minutes. To this mixture were added S-PHOS (96 mg, 0.234 mmol, CAS RN 657408-07-6) and Pd(PPh3)4 (44 mg, 0.046 mmol), degassed for another 15 minutes, and heated to 90° C. for 1 h in microwave. Work up and purification as described in example 25 yielded 15 mg of the title compound. Off-white solid (7%). MS (ESI): m/z=487.0 [M+H]+.

WORKUP

后处理

  1. customdegassed for another 15 minutes
  2. custompurification