Réaction #1095910

Équation de réaction

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

Rendement 97.2%

Solvants

acetonitrile

Conditions de réaction

Traitement

1. 1
   TempératureThe reaction mixture was cooled to near room temperature
2. 2
   Extractionthe mixture was extracted with tert-butyl methyl ether three times
3. 3
   LavageThe organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   Séchagedried over anhydrous magnesium sulfate
5. 5
   Concentrationconcentrated

Mode opératoire

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.

Source