HRID661622

反应详情

EQUATION

反应方程式

HRID 661622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of dioxane (1.0 mL) containing 3-bromo-4-chloro-N-[2-(2-dimethylamino-ethoxy)-phenyl]-N-methyl-benzamide (44.0 mg, 0.11 mmol), Pd2(dba)3 (10 mg, 0.01 mmol), P(t-Bu)3HBF4 (7 mg, 0.022 mmol), KF (22 mg, 0.38 mmol) and 2,4 dichloropyridine-5-boronic acid (21 mg, 0.11 mmol) was degassed by bubbling N2 for 5 minutes and then sealed and heated at 110° C. overnight. The mixture was filtered and purified by preparative LCMS to yield 4-chloro-3-(4,6-dichloro-pyridin-3-yl)-N-[2-(2-dimethylamino-ethoxy)-phenyl]-N-methyl benzamide 7-1. MS [M+H]+: 478.0; tR=5.26 min. (method 2)

WORKUP

后处理

  1. customwas degassed
  2. customby bubbling N2 for 5 minutes
  3. customsealed
  4. filtrationThe mixture was filtered
  5. custompurified by preparative LCMS