Reaktion #1095912

Reaktionsgleichung

ammonium chloride

4,6-dichloro-5-fluoropyrimidine

potassium carbonate

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

→

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

Ausbeute 97.2%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was cooled to near room temperature
2. 2
   Extraktionthe mixture was extracted with tert-butyl methyl ether three times
3. 3
   WaschenThe organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   Trocknendried over anhydrous magnesium sulfate
5. 5
   Einengenconcentrated

Vorschrift

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 cis-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 0.3 g of 1-(6-chloro-5-fluoropyrimidin-4-yl)-cis-2,6-dimethylhexahydro-1H-azepine

Quelle