反应详情

A mixture of 1.0 g of 9-(2-hydroxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one, 2 ml of triethylamine and 2 ml of acetic anhydride in 20 ml of toluene is kept on a water bath at 80°-85° C. for 3 hours. After cooling, to the mixture is added water, the organic layer is collected by a separatory funnel and concentrated. To the residue is added hexane and the precipitated crystals are collected by filtration. The resulting crystals are recrystallized from isopropyl ether to give 0.5 g of 9-(2-acetoxyethyl)-4,4a,5,6-tetrahydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one as white crystals, melting at 106°-108° C.

1. temperatureAfter cooling, to the mixture
2. customthe organic layer is collected by a separatory funnel
3. concentrationconcentrated
4. additionTo the residue is added hexane
5. filtrationthe precipitated crystals are collected by filtration
6. customThe resulting crystals are recrystallized from isopropyl ether