반응 #42851

반응 방정식

ammonium chloride

4,6-dichloro-5-fluoropyrimidine

potassium carbonate

trans-2,6-dimethylhexahydro-1H-azepine hydrochloride

→

1-(6-chloro-5-fluoropyrimidin-4-yl)-trans-2,6-dimethylhexahydro-1H-azepine

수율 100.4%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to near room temperature
2. 2
   추출the mixture was extracted with tert-butyl methyl ether three times
3. 3
   세척The organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   농축concentrated

실험 절차

Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloro-5-fluoropyrimidine, 0.50 g of potassium carbonate and 0.27 g of trans-2,6-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 2 hours at 60° 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 0.31 g of 1-(6-chloro-5-fluoropyrimidin-4-yl)-trans-2,6-dimethylhexahydro-1H-azepine.

출처