반응 #1702109

반응 방정식

3-methoxybenzylamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

수율 93.2%

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

수율 93.2%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The reaction was quenched with water
2. 2
   workup.ADDITIONEthyl acetate (“EtOAc”) was added
3. 3
   기타the layers were separated
4. 4
   추출The aqueous layer was extracted with EtOAc once
5. 5
   세척The combined organic layers were washed with water and brine successively
6. 6
   건조dried (Na2SO4)
7. 7
   여과filtered
8. 8
   농축concentrated
9. 9
   기타The crude product was purified by silica gel column chromatography

실험 절차

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.

출처