反应 #1702146

反应方程式

2,5-dichloro-N-[3-(3-methoxyphenyl)propyl]pyrimidin-4-amine

2,5-Dichloro-N-[3-(3-methoxyphenyl)propyl]pyrimidin-4-amine

2-(3-aminophenyl)ethanol

2-(3-Aminophenyl)ethanol

p-toluenesulfonic acid monohydrate

→

desired product

收率 92.3%

2-{3-[(5-Chloro-4-{[3-(3-methoxyphenyl)propyl]amino}pyrimidin-2-yl)amino]phenyl}ethanol

收率 92.3%

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 and H2O successively

实验过程

To a solution of 2,5-dichloro-N-[3-(3-methoxyphenyl)propyl]pyrimidin-4-amine (0.50 g, 1.6 mmol) (prepared according to Example 10, Step A) and 2-(3-aminophenyl)ethanol (0.30 g, 2.2 mmol) (prepared according to Example 2, Step A) in 1,4-dioxane (13.6 mL) was added p-toluenesulfonic acid monohydrate (0.11 g, 0.58 mmol). The mixture was heated at 100° C. for 16 hours and the reaction was complete. After cooling, the mixture was filtered under vacuum. The cake was washed with cold EtOAc and H2O successively to give the desired product as a light brown gum (0.61 g, 92%). LCMS for C22H26ClN4O2 (M+H)+: m/z=413.1.

来源