Potassium Carbonate → FK 360

関与物質

反応手順

To a mixture of 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxylic acid (5 g), dichloromethane (45 ml) and N,N-dimethylformamide (11 ml), thionyl chloride (2.1 g) was added at 7° C. under ice cooling. After stirring for 1.5 hours at the same condition, to a solution of N-methylpiperazine (3.7 g) in dichloromethane (37 ml), the reaction mixture was added under ice cooling and stirred for 2 hours. The reaction mixture was adjusted to pH=8.5 by saturated potassium carbonate and extracted with chloroform. The organic layer was washed with water and brine and dried over magnesium sulfate. The solvent was distilled off to give a residue, which was chromatographed on alumina eluting with a chloroform. The fractions containing the desired product were combined and concentrated in vacuo. The crystalline residue was recrystallized from diethyl ether to afford 6-methyl-5-(4-methylpiperazin-1-ylcarbonyl)-4-(3-nitrophenyl)-2-phenyl-pyrimidine (3.5 g).

情報源と証拠