反应详情

Dibenzo[b,f][1,4]oxazepin-11(10H)-one (1.001 g, 4.7 mmol) was dissolved in THF (20 mL) and the borane (2M in THF, 20 mL, 40.0 mmol) was added. The reaction mixture was refluxed for 3 hours. The mixture was cooled down to room temperature and an excess of ethanol was added to quench the reaction. The resulting mixture was refluxed for 2 hours. The mixture was cooled down and concentrated in vacuo. The residue was dissolved in ethyl acetate and the organic layer was washed with water and brine, dried over sodium sulfate, filtered and evaporated to afford title compound 398 (0.945 g, quantitative). MS (m/z): 198.1 (M+H). 1H NMR (CD3OD) δ (ppm): 7.29-7.19 (m, 2H), 7.16-7.04 (m, 2H), 7.01-6.99 (m, 1H), 6.82-6.78 (m, 1H), 6.63-6.59 (m, 2H), 4.88 (s, 1H), 4.39 (s, 2H). MS (m/z): 198.1 (M+H).

1. temperatureThe reaction mixture was refluxed for 3 hours
2. customto quench
3. customthe reaction
4. temperatureThe resulting mixture was refluxed for 2 hours
5. temperatureThe mixture was cooled down
6. concentrationconcentrated in vacuo
7. dissolutionThe residue was dissolved in ethyl acetate
8. washthe organic layer was washed with water and brine
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. customevaporated