反应详情

温度

0 °C

A mixture of 2-amino-5-phenyl-1,3,4-thiadiazole sulphate (10.0 g, 56.4 mmol) and conc. hydrochloric acid (100 ml) was stirred at 0° C. Sodium nitrite (5.06 g, 69 mmol) was added at 0° C. The mixture was stirred for 9 days at room temperature. The crystals were filtered and resuspended in aqueous hydrochloric acid (150 ml, 1M), stirred overnight and filtered. Aqueous sodium hydroxide (100 ml, 4 M) was added and extracted with ethyl acetate. Yield 5.68 g.

1. stirringThe mixture was stirred for 9 days at room temperature
2. filtrationThe crystals were filtered
3. stirringstirred overnight
4. filtrationfiltered
5. additionAqueous sodium hydroxide (100 ml, 4 M) was added
6. extractionextracted with ethyl acetate