反应详情

To 15 ml of dimethylformamide were dissolved 3,5-dinitrobenzoyl chloride (2.5 g) and 1,3-thiazolidine-2-thione (1.3 g). To the solution was added dropwise a solution of triethyl amine (1.2 g) and dimethylformamide (2 ml) under ice-cooling. The mixture was stirred under ice-cooling for 1 hour and at room temperature for 5 hours. The reaction mixture was filtered and the solvent was removed at a reduced pressure. To the residue was added water and the insolubles were filtered off. The filtrate was washed with cold methanol and then with ether to obtain crude crystals. Recrystallization from toluene gives 2.4 g of the desired compound as yellow needle crystals (yield 76.7%).

1. temperaturecooling
2. filtrationThe reaction mixture was filtered
3. customthe solvent was removed at a reduced pressure
4. additionTo the residue was added water
5. filtrationthe insolubles were filtered off
6. washThe filtrate was washed with cold methanol
7. customwith ether to obtain crude crystals
8. customRecrystallization from toluene