反应 #1702156

反应方程式

1-(3-bromo-5-methoxyphenyl)methanamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

收率 87.0%

N-(3-Bromo-5-methoxybenzyl)-2,5-dichloropyrimidin-4-amine

收率 87.0%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   其他The reaction mixture was quenched with water
2. 2
   workup.ADDITIONEtOAc was added
3. 3
   其他the layers were separated
4. 4
   萃取The aqueous layer was extracted with EtOAc twice
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 residue was purified by silica gel column chromatography

实验过程

To a solution of 1-(3-bromo-5-methoxyphenyl)methanamine (2.57 g, 11.9 mmol) and 2,4,5-trichloropyrimidine (2.4 g, 13 mmol) in N,N-dimethylformamide (30 mL) was added potassium carbonate (3.3 g, 24 mmol). The resultant mixture was stirred overnight at room temperature. The reaction mixture was quenched with water. EtOAc was added and the layers were separated. The aqueous layer was extracted with EtOAc twice. The combined organic layers were washed with water and brine successively, then dried (Na2SO4), filtered, and concentrated. The residue was purified by silica gel column chromatography to give the desired product (3.7 g, 87%). LCMS for C12H10BrCl2N3O (M+H)+: m/z=361.9, 363.9.

来源