反应详情

15.3 g of N-methyl-(7-isopropoxycarbonyl-6-methyl-2,3,5,6-tetrahydropyrrolo[2,1-b]thiazol-3-ylidene)acetamide was dissolved in a solvent mixture comprising 300 ml of chloroform and 120 ml of tetrahydrofuran. Then 11.7 g of 2,3-dichloro-5,6-dicyano-parabenzoquinone was added thereto under stirring and cooling with cold water. After 0.5 hour, a saturated aqueous solution of sodium hydrogencarbonate was added thereto. After stirring, the insoluble matters were filtered off with the use of celite and the filtrate was extracted with chloroform. The chloroform phase was washed with water and a saturated aqueous solution of sodium chloride and dried. After distilling off the solvent, the obtained crude crystals were recrystallized from ethanol. Thus 12.5 g of the title compound was obtained.

1. stirringAfter stirring
2. filtrationthe insoluble matters were filtered off with the use of celite
3. extractionthe filtrate was extracted with chloroform
4. washThe chloroform phase was washed with water
5. dry with materiala saturated aqueous solution of sodium chloride and dried
6. distillationAfter distilling off the solvent
7. customthe obtained crude crystals
8. customwere recrystallized from ethanol