Triethylamine → HCID 178430504、化合物

関与物質

反応手順

1.5 g (7.0 mmol) of 1-(4-chlorobutyl)-4-hydroxy-5-methylpyrimidin-2(1H)-one from Example 5.2.1, 2.0 g (7.0 mmol) of 2-tert-butyl-4-piperazin-1-yl-6-(trifluoromethyl)pyrimidine (DE 197 35 410) and 1.4 g (14.0 mmol) of NEt3 in 100 ml of N,N-dimethylformamide (DMF) were stirred at 110° C. for 24 hours. Then ethyl acetate was added, and the mixture was washed twice with water. The combined organic phases were dried over Na2SO4, filtered to remove the desiccant and concentrated in vacuo. The oily residue was purified by chromatography on silica gel (eluent: dichloromethane:methanol 95:5 v/v), and stirred with pentane and filtered off with suction. The solid was taken up in a little methylene chloride, and a solution of HCl in diethyl ether was added, whereupon the required product precipitated as hydrochloride. The hydrochloride was filtered off with suction and washed with diethyl ether, and the title compound was dried in vacuo at 40° C. Yield: 1.1 g.

情報源と証拠