تفاعل #1702134

معادلة التفاعل

3-(3-methoxyphenyl)propan-1-amine hydrochloride

2,4,5-trichloropyrimidine

potassium carbonate

→

desired product

المردود 91.1%

2,5-Dichloro-N-[3-(3-methoxyphenyl)propyl]pyrimidin-4-amine

المردود 91.1%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction was quenched with water
2. 2
   workup.ADDITIONEtOAc was added
3. 3
   أخرىthe layers were separated
4. 4
   استخلاصThe aqueous layer was extracted with EtOAc twice
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
   أخرىthen triturated with cold EtOAc)

الإجراء التجريبي

To a solution of 3-(3-methoxyphenyl)propan-1-amine hydrochloride (2.00 g, 9.92 mmol) and 2,4,5-trichloropyrimidine (1.19 mL, 10.4 mmol) in N,N-dimethylformamide (30 mL) was added potassium carbonate (4.80 g, 34.7 mmol). The resultant mixture was stirred overnight at room temperature. The reaction 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 (then triturated with cold EtOAc) to give the desired product as a light brown gel (2.82 g, 91%). LCMS for C14H16Cl2N3O (M+H)+: m/z=312.0, 314.0.

المصدر