反应详情

温度

20 °C

Butyric acid (0.71 g.) is added to a suspension of 6-(7-chloro-1,8-naphthyridin-2-yl)-7-oxo-5-(piperazin-1-yl)carbonyloxy-2,3,6,7-tetrahydro-5H-1,4-dithiino[2,3-c]pyrrole (2.50 g.) and N,N'-dicyclohexyl-carbodiimide (1.67 g.) in anhydrous methylene chloride (50 cc.) and the mixture is stirred for 1 hour at 20° C. After filtering off the dicyclohexylurea formed, washing with methylene chloride (15 cc.) and evaporating the solvent, the residue obtained (3.8 g.) is washed with boiling ethanol (35 cc.) and then recrystallised from a mixture of acetonitrile (110 cc.) and ethanol (11 cc.). 5-(4-Butyrylpiperazin-1-yl)carbonyloxy-6-(7-chloro-1,8-naphthyridin-2-yl)-7-oxo-2,3,6,7-tetrahydro-5H-1,4-dithiino[2,3-c]pyrrole (1.95 g.), which melts at 248° C., is thus obtained.

1. filtrationAfter filtering off the dicyclohexylurea
2. customformed
3. washwashing with methylene chloride (15 cc.)
4. customevaporating the solvent
5. customthe residue obtained (3.8 g.)
6. washis washed with boiling ethanol (35 cc.)
7. customrecrystallised from a mixture of acetonitrile (110 cc.) and ethanol (11 cc.)