تفاعل #42848

معادلة التفاعل

ammonium chloride

4,6-dichloro-5-fluoropyrimidine

potassium carbonate

2,5-dimethylhexahydro-1H-azepine hydrochloride

→

1-(6-chloro-5-fluoro pyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine

المردود 97.2%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture was cooled to near room temperature
2. 2
   استخلاصthe mixture was extracted with tert-butyl methyl ether three times
3. 3
   غسيلThe organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   تركيزconcentrated

الإجراء التجريبي

Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloro-5-fluoropyrimidine, 0.50 g of potassium carbonate and 0.24 g of 2,5-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 5 hours at 80° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.3 g of 1-(6-chloro-5-fluoro pyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine.

المصدر