反应详情

温度

70 °C

A mixture of 3,4-dichloro-1,2,5-thiadiazole (4.00 g, 25.8 mmol) and piperazine hexahydrate (25.0 g, 130 mmol) in DMF (25 mL) was heated at 70° C. for 20 minutes. After cooling to ambient temperature, the reaction mixture was basified (11 M NaOH) and brine was added. The resulting mixture was extracted with CHCl3 (×3). The combined organic phases were washed twice with brine/water (1:1), dried (MgSO4) and the solvent was evaporated. The resulting oil was purified by column chromatography on silica gel using CHCl3 as eluent to give 2.77 g (52%) of the title compound as a colourless oil which was converted to its hydrochloride salt: mp 231° C. (dec). Anal (C6H9ClN4S.HCl), C calc 29.89, found 30.4. H. N

1. temperatureAfter cooling to ambient temperature
2. additionwas added
3. extractionThe resulting mixture was extracted with CHCl3 (×3)
4. washThe combined organic phases were washed twice with brine/water (1:1)
5. dry with materialdried (MgSO4)
6. customthe solvent was evaporated
7. customThe resulting oil was purified by column chromatography on silica gel