反应详情

温度

140 °C

In a dried flask under an inert atmosphere, 103 mg (0.36 mmol) of 8-(3-fluoro-benzyloxy)-1,3-dihydro-benzo[d]azepin-2-one and 72 mg (0.9 mmol) of sodium acetate were suspended in 0.3 ml of acetic acid anhydride. The solution was heated to 140° C. for 4 h. For the working-up, the reaction mixture was cooled, then evaporated under reduced pressure. The residue was treated with 1.5 ml of ice/water and 4 ml of ethyl acetate. The aqueous layer was separated and re-extracted with 4 ml of ethyl acetate. The combined organic layers were dried over sodium sulfate, thereafter the solvent evaporated under reduced pressure. For purification, the crude material obtained was chromatographed on silica gel using a gradient of heptane to a 4:1-mixture of heptane and ethyl acetate as the eluent. There were obtained 91 mg (77% of theory) of 3-acetyl-8-(3-fluoro-benzyloxy)-1,3-dihydro-benzo[d]azepin-2-one as a light yellow solid; MS: m/e=325 (M)+.

1. temperaturethe reaction mixture was cooled
2. customevaporated under reduced pressure
3. additionThe residue was treated with 1.5 ml of ice/water and 4 ml of ethyl acetate
4. customThe aqueous layer was separated
5. extractionre-extracted with 4 ml of ethyl acetate
6. dry with materialThe combined organic layers were dried over sodium sulfate
7. customthe solvent evaporated under reduced pressure
8. customFor purification
9. customthe crude material obtained
10. customwas chromatographed on silica gel using a gradient of heptane to a 4