反応 #1702109

反応方程式

3-methoxybenzylamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

収率 93.2%

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

収率 93.2%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   その他The reaction was quenched with water
2. 2
   workup.ADDITIONEthyl acetate (“EtOAc”) was added
3. 3
   その他the layers were separated
4. 4
   抽出The aqueous layer was extracted with EtOAc once
5. 5
   洗浄The combined organic layers were washed with water and brine successively
6. 6
   乾燥dried (Na2SO4)
7. 7
   ろ過filtered
8. 8
   濃縮concentrated
9. 9
   その他The crude product was purified by silica gel column chromatography

実験手順

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.

出典