反应 #1702157

反应方程式

NaHCO3

N-(3-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 99.0%

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

收率 99.0%

溶剂

1,4-dioxane

反应条件

后处理

1. 1
   其他After removal of the organic solvent
2. 2
   萃取the aqueous layer was extracted with methylene chloride twice
3. 3
   洗涤The combined organic layers were washed with water and brine successively
4. 4
   干燥dried (Na2SO4)
5. 5
   过滤filtered
6. 6
   浓缩concentrated

实验过程

Into a reaction flask were added N-(3-bromo-5-methoxybenzyl)-2,5-dichloropyrimidin-4-amine (2.0 g, 5.5 mmol), 1,4-dioxane (30 mL), 3-(3-aminophenyl)propan-1-ol (1.2 g, 8.3 mmol, prepared according to Example 12, Step B), and p-toluenesulfonic acid monohydrate (0.12 g, 0.63 mmol). The mixture was heated at 70° C. over two days and NaHCO3 (saturated aqueous solution) was added. After removal of the organic solvent, the aqueous layer was extracted with methylene chloride twice. The combined organic layers were washed with water and brine successively, then dried (Na2SO4), filtered, and concentrated to give the desired product as a white powder (2.6 g, 99%). LCMS for C21H22BrClN4O2 (M+H)+: m/z=477.0, 479.0.

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