反应详情

To a solution of 0.82 g (4 mmol) of 5H,7H-dibenzo[b,d]azepin-6-one in 15 ml of dimethylformamide at room temperature 0.20 g (5 mmol) of sodium hydride 55% in oil was added. After stirring for 30 min at room temperature 0.75 g (5 mmol) of p-methoxybenzyl chloride were added and stirring was continued at room temperature for 2 hours. For workup the mixture was distributed between water and ethyl acetate. The organic layer was re-extracted with 1 N hydrochloric acid and the aqueous layers were washed with ethyl acetate. The combined organic layers were dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography (hexane/ethyl acetate=1:1) to yield 1.175 g (91%) of 5-(4-methoxybenzyl)-5H,7H-dibenzo[b,d]azepin-6-one as a colourless oil; MS: m/e: 330.4 (M+H+).

1. additionwere added
2. extractionThe organic layer was re-extracted with 1 N hydrochloric acid
3. washthe aqueous layers were washed with ethyl acetate
4. dry with materialThe combined organic layers were dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography (hexane/ethyl acetate=1:1)