反应详情

In 30 ml of dichloromethane was suspended 21.0 g of 2-(4-chloro-2-fluorophenyl)-3-hydroxy-2,3,4,5,6,7-hexahydro-1H-isoindol-1-one, and 7.5 ml of thionyl chloride was added to the suspension under stirring over a 20-minute period. The reaction mixture was warmed, stirred at 40° to 45° C. for 1 hour and concentrated to dryness under reduced pressure. The residue was dissolved in methylene chloride and, upon addition of hexane, there was produced insoluble matter, which was filtered out. The filtrate was concentrated to dryness under reduced pressure, thereby affording 19.5 g (yield of 87%) of crystals of the subject compound. Recrystallization from cyclohexane yielded white crystals, m.p. 89°-90° C.

1. additionwas added to the suspension
2. temperatureThe reaction mixture was warmed
3. stirringstirred at 40° to 45° C. for 1 hour
4. concentrationconcentrated to dryness under reduced pressure
5. dissolutionThe residue was dissolved in methylene chloride and, upon addition of hexane
6. customthere was produced insoluble matter, which
7. filtrationwas filtered out
8. concentrationThe filtrate was concentrated to dryness under reduced pressure