反应详情

A suspension of 8-methoxy-2-oxo-2,3,4,5-tetrahydro-1H-3-benzazepine (20.4 g, 0.105 m) in tetrahydrofuran (500 ml) was added to 1 M borane in tetrahydrofuran (300 ml) stirred at 5°. The mixture was heated to reflux for 2 hours, cooled, treated with 3N hydrochloric acid (300 ml), concentrated in vacuo to remove tetrahydrofuran and heated to reflux for 1 hour. The mixture was concentrated in vacuo, filtered and the filter cake was dissolved in methanol, heated to reflux, dried with magnesium sulfate and concentrated in vacuo to afford 7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride, m.p. 229°-231°.

1. temperatureThe mixture was heated
2. temperatureto reflux for 2 hours
3. temperaturecooled
4. concentrationconcentrated in vacuo
5. customto remove tetrahydrofuran
6. temperatureheated
7. temperatureto reflux for 1 hour
8. concentrationThe mixture was concentrated in vacuo
9. filtrationfiltered
10. dissolutionthe filter cake was dissolved in methanol
11. temperatureheated
12. temperatureto reflux
13. dry with materialdried with magnesium sulfate
14. concentrationconcentrated in vacuo