反应详情

A solution of 3.7 g of 4-oxo-4,5,6,7-tetrahydrothieno-[2,3-b]thiepin-5-acetic acid and 2.6 g of 4-chlorophenylhydrazine in 50 ml of ethanol is refluxed under heating for 6.5 hours. Then, the reaction mixture is concentrated under reduced pressure. The resulting residue is dissolved in 40 ml of acetic acid and the solution is refluxed under heating fo 1.5 hours. After cooling, the reaction mixture is concentrated under reduced pressure, the residue is subjected to column chromatography on silica gel and eluted with chloroform. The crystals obtained from the fraction are recrystallized from a mixed solvent of chloroform and ethanol to give 1.7 g of 2-(4-chlorophenyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one as pale brown crystals, melting at 134°-135° C.

1. temperatureunder heating for 6.5 hours
2. concentrationThen, the reaction mixture is concentrated under reduced pressure
3. dissolutionThe resulting residue is dissolved in 40 ml of acetic acid
4. temperaturethe solution is refluxed
5. temperatureunder heating
6. temperatureAfter cooling
7. concentrationthe reaction mixture is concentrated under reduced pressure
8. washeluted with chloroform
9. customThe crystals obtained from the fraction
10. customare recrystallized from a mixed solvent of chloroform and ethanol