反应详情

温度

50 °C

To a solution of 4-nitrobenzoyl chloride (3.1 g) and tetrahydrofuran (50 ml) were added 1,3-thiazolidine-2-thione (2.0 g) and triethyl amine (2.5 g). The mixture was stirred at 50° C. for 30 minutes under nitrogen atmosphere. The reaction mixture was filtered and the solvent was removed at a reduced pressure. To the residue was added water, and the solution is extracted with dichloromethane. The extract was washed with a saturated aqueous solution of sodium chloride and dried with use of Glauber's salt. The solvent was distilled off and the resulting crystals were purified by silica gel column chromatography (developer: dichloromethane) and recrystallized from dichloromethane to obtain 3.3 g of the desired compound as yellow needle crystals (yield 82.5%).

1. filtrationThe reaction mixture was filtered
2. customthe solvent was removed at a reduced pressure
3. additionTo the residue was added water
4. extractionthe solution is extracted with dichloromethane
5. washThe extract was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried with use of Glauber's salt
7. distillationThe solvent was distilled off
8. customthe resulting crystals were purified by silica gel column chromatography (developer: dichloromethane)
9. customrecrystallized from dichloromethane