反应详情

To a solution of 1.50 g of 2,5-dimercapto-1,3,4-thiadiazole and 4.2 ml of triethylamine in 30 ml of DMF was added 1.29 g of α-chloroacetamidine hydrochloride at room temperature under stirring. Further, the mixture was stirred for 2.5 hours at room temperature and concentrated under reduced pressure. The residue was subjected to a column chromatography on silica gel (100 g), eluting with a (4:1) mixture of acetonitrile and water. The pertinent fractions were collected and concentrated under reduced pressure, and the concentrate was subjected to a column chromatography on XAD-II (450 ml) being washed with water, and eluted with 10% aqueous ethanol. After concentrating, the precipitating crystals were filtered to give 755mg of 2-amidinomethylthio-5-mercapto-1,3,4-thiadiazole as colorless crystals, mp: 184°-187° C.

1. stirringFurther, the mixture was stirred for 2.5 hours at room temperature
2. concentrationconcentrated under reduced pressure
3. washeluting with a (4:1) mixture of acetonitrile and water
4. customThe pertinent fractions were collected
5. concentrationconcentrated under reduced pressure
6. washbeing washed with water
7. washeluted with 10% aqueous ethanol
8. concentrationAfter concentrating
9. filtrationthe precipitating crystals were filtered