反应详情

To a solution of 5.37 g of (E)-N-cinnamyl-N'-(3-pyridyl)ethylenediamine dissolved in 100 ml of tetrahydrofuran, 4.5 g of triethylamine was added and the mixture was ice-cooled. To the mixture was added dropwise 20 ml of a tetrahydrofuran solution containing 5.12 g of thiophosgene over 5 minutes, and subsequently the mixture was stirred under ice-cooling for 30 minutes and then at room temperature for 2 hours. The solvent was distilled off, and the residue was dissolved in chloroform, washed with water and dried, followed by distillation of the solvent. The residue was purified by silica gel column chromatorgraphy (solvent: chloroform-methanol=20:1) to give 2.86 g of (E)-1-cinnamyl-3-(3-pyridyl)imidazolidine-2-thione as caramel.

1. temperaturecooled
2. temperaturecooling for 30 minutes
3. distillationThe solvent was distilled off
4. dissolutionthe residue was dissolved in chloroform
5. washwashed with water
6. customdried
7. distillationfollowed by distillation of the solvent
8. customThe residue was purified by silica gel column chromatorgraphy (solvent: chloroform-methanol=20:1)