反应 #1702138

反应方程式

(1S)-1-(3-methoxyphenyl)ethanamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

收率 96.0%

2,5-Dichloro-N-[(1S)-1-(3-methoxyphenyl)ethyl]pyrimidin-4-amine

收率 96.0%

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.ADDITIONThen EtOAc 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
6. 6
   干燥dried (Na2SO4)
7. 7
   过滤filtered
8. 8
   浓缩concentrated

实验过程

To a solution of (1S)-1-(3-methoxyphenyl)ethanamine (1.50 g, 9.92 mol) (S-isomer, >99% ee purity) and 2,4,5-trichloropyrimidine (1.19 mL, 10.4 mmol) in N,N-dimethylformamide (30 mL) was added potassium carbonate (4.1 g, 30 mmol). The resultant mixture was stirred overnight at room temperature. The reaction was quenched with water. Then 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 then dried (Na2SO4), filtered, and concentrated to give the desired product as a light yellow thick oil (2.84 g, 96%). LCMS for C13H14Cl2N3O (M+H)+: m/z=298.0, 300.0, 302.0 (9:6:1).

来源