反应详情

To a solution of adamantane-1-carboxylic acid chloride (1.09 g, 0.005 mol) in dichloromethane (25 mL) was added N-(1-methylethyl)-2-[4-(2-pyrimidinyl)-1-piperazinyl]ethylamine (1.27 g, 0.005 mol) in dichloromethane (15 mL) and triethylamine (2.0 mL, 0.014 mol) at room temperature. The resulting solution was stirred at room temperature for 2 days. The reaction mixture was then washed with water (50 mL), dried over anhydrous magnesium sulfate, and concentrated on a rotary evaporator. The desired product (TLC on silica gel using 30% methanol/ethyl acetate as eluant, Rf=0.51) was isolated by chromatography on 200 g of silica gel using 30% methanol/ethyl acetate and converted to the dihydrochloride salt with isopropanolic HCl (1.87 g, 76%); mp=194°-196° C.

1. washThe reaction mixture was then washed with water (50 mL)
2. dry with materialdried over anhydrous magnesium sulfate
3. concentrationconcentrated on a rotary evaporator