تفاعل #1702109

معادلة التفاعل

3-methoxybenzylamine

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

المردود 93.2%

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

المردود 93.2%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction was quenched with water
2. 2
   workup.ADDITIONEthyl acetate (“EtOAc”) was added
3. 3
   أخرىthe layers were separated
4. 4
   استخلاصThe aqueous layer was extracted with EtOAc once
5. 5
   غسيلThe combined organic layers were washed with water and brine successively
6. 6
   تجفيفdried (Na2SO4)
7. 7
   ترشيحfiltered
8. 8
   تركيزconcentrated
9. 9
   أخرىThe crude product was purified by silica gel column chromatography

الإجراء التجريبي

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.

المصدر