Reaction #3501093
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08129526B2
Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: Into 2 ml of acetnitrile were added 0.13 g of 4,6-dichloro-5-fluoropyrimidine, 0.14 g of potassium carbonate and 0.10 g of 2-methylhexahydro-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 0.20 g of 1-(6-chloro-5-fluoropyrimidin-4-yl)-2-methylhexahydro-1H-azepine. The reaction mixture was cooled to near room temperature 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 concentrated
Source ID: ord-041702dba85249c2beb753dc1033c463