反应 #1702151

反应方程式

N-(2-bromo-5-methoxybenzyl)-2,5-dichloropyrimidin-4-amine

3-(3-aminophenyl)propan-1-ol

3-(3-Aminophenyl)propan-1-ol

p-toluenesulfonic acid monohydrate

→

desired product

收率 83.0%

3-[3-({4-[(2-Bromo-5-methoxybenzyl)amino]-5-chloropyrimidin-2-yl)amino]phenyl}propan-1-ol

收率 83.0%

溶剂

1,4-dioxane

反应条件

后处理

1. 1
   温度After cooling
2. 2
   过滤the mixture was filtered under vacuum
3. 3
   洗涤The cake was washed with cold EtOAc

实验过程

To a solution of N-(2-bromo-5-methoxybenzyl)-2,5-dichloropyrimidin-4-amine (4.0 g, 11 mmol) and 3-(3-aminophenyl)propan-1-ol (2.3 g, 15 mmol, prepared according to Example 12, Step B) in 1,4-dioxane (90 mL) was added p-toluenesulfonic acid monohydrate (0.31 g, 1.6 mmol). The mixture was heated at 80° C. over two days and the reaction was complete. After cooling, the mixture was filtered under vacuum. The cake was washed with cold EtOAc to give the desired product as an off-white powder (4.35 g, 83%). LCMS for C21H22BrClN4O2 (M+H)+: m/z=477.0, 479.0.

来源