反应详情

To a mixture of 4-methyl-2-(3-nitrophenyl)-6-phenyl-3-pyridinecarboxylic acid (1.4 g), methylene chloride 14 ml) and N,N-dimethylformamide (2.8 ml) was added a solution of thionyl chloride (0.33 ml) in methylene chloride (3 ml) at 7° C. under ice cooling. After stirring for 2 hours at the same condition, a solution of 1-methylpiperazine (1.05 g) in methylene chloride (7 ml) was added thereto and the mixture was stirred for 2 hours at the same temperature. After adding Water (100 ml) and methylene chloride (50 ml) thereto, the mixture was adjusted to pH 8.5 with 10% aqueous sodium hydroxide. The organic layer was separated, washed successively with water and saturated brine, dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from a mixture of ethanol and diethyl ether to give 4-methyl-3-(4 methylpiperazin-1-ylcarbonyl)-2-(3-nitrophenyl)-6-phenylpyrid ine (0.97 g).

1. stirringthe mixture was stirred for 2 hours at the same temperature
2. customThe organic layer was separated
3. washwashed successively with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue was recrystallized from a mixture of ethanol and diethyl ether