反应 #1702109

反应方程式

3-methoxybenzylamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

收率 93.2%

2,5-Dichloro-N-(3-methoxybenzyl)pyrimidin-4-amine

收率 93.2%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他The reaction was quenched with water
2. 2
   workup.ADDITIONEthyl acetate (“EtOAc”) was added
3. 3
   其他the layers were separated
4. 4
   萃取The aqueous layer was extracted with EtOAc once
5. 5
   洗涤The combined organic layers were washed with water and brine successively
6. 6
   干燥dried (Na2SO4)
7. 7
   过滤filtered
8. 8
   浓缩concentrated
9. 9
   其他The crude product was purified by silica gel column chromatography

实验过程

To a solution of 3-methoxybenzylamine (0.75 g, 5.4 mmol) and 2,4,5-trichloropyrimidine (1.1 g, 6.0 mmol) in N,N-dimethylformamide (20 mL) was added potassium carbonate (2.3 g, 16 mmol). The resulting mixture was stirred overnight at room temperature. The reaction was quenched with water. Ethyl acetate (“EtOAc”) was added and the layers were separated. The aqueous layer was extracted with EtOAc once. The combined organic layers were washed with water and brine successively, then dried (Na2SO4), filtered, and concentrated. The crude product was purified by silica gel column chromatography to give the desired product as a white powder (1.43 g, 92%). LCMS for C12H12ClN3O (M+H)+: m/z=284.0, 286.0.

来源