反应详情

A solution of hydrogen chloride in methanol (225 ml) was added to a suspension of 3-(2-t-butoxycarbonyl-2-methylhydrazinomethylene)-6-chloro-2,3-dihydro-4H-1-benzothiopyran-4-one (54.14 g) in methanol (550 ml). After being stirred at ambient temperature for 8 hours, the mixture was evaporated in vacuo and the residue was extracted with ethyl acetate after an addition of water. The extract was washed with aqueous sodium bicarbonate and then water, dried over magnesium sulfate, and evaporated in vacuo to give 8-chloro-1-methyl-1,4-dihydro[1]benzothiopyrano[4,3-c]pyrazole (26.63 g).

1. customthe mixture was evaporated in vacuo
2. extractionthe residue was extracted with ethyl acetate
3. additionafter an addition of water
4. washThe extract was washed with aqueous sodium bicarbonate
5. dry with materialwater, dried over magnesium sulfate
6. customevaporated in vacuo