反应详情

Thieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.5 g) was suspended in 1,2-dichloroethane (20 ml) and propionyl chloride (770 mg) was added. To this reaction system was added portionwise aluminum chloride (4.7 g) under ice-cooling. Insoluble matter was filtrated, and the filtrate was poured into ice water and chloroform was added. The aqueous layer was extracted twice with chloroform and the combined organic layer was dried over sodium sulfate. The solvent was evaporated under reduced pressure and the precipitated crystals were collected by filtration to give 2-propionylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.4g).

1. temperaturecooling
2. filtrationInsoluble matter was filtrated
3. additionthe filtrate was poured into ice water and chloroform
4. additionwas added
5. extractionThe aqueous layer was extracted twice with chloroform
6. dry with materialthe combined organic layer was dried over sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. filtrationthe precipitated crystals were collected by filtration