反应详情

温度

5 °C

3,4-Dinitrobenzoic acid (50 g, (124 mol) was heated at reflux in SOCl2 (160 ml) for 6 hours. The mixture was then evaporated to dryness in vacuo. The product was dissolved in THF and cooled to 5° C. To this solution, N-methylpiperazine (26.2 ml, 0.24 mol) and Et3N (42 ml) were added dropwise as a solution in THF (50 ml). After stirring overnight at room temperature, the solution was poured into water (1.5 L) and stirred at approximately 5° C. for 0.5 hours. The solid precipitate which formed was collected and dried to give (3,4-dinitrophenyl)-(4-methylpiperazin-1-yl)-methanone (40 g) as a yellow solid.

1. customThe mixture was then evaporated to dryness in vacuo
2. dissolutionThe product was dissolved in THF
3. stirringstirred at approximately 5° C. for 0.5 hours
4. customThe solid precipitate which formed
5. customwas collected
6. customdried