反应详情

A mixture of 9-chloro-8-fluoro-4-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (1 equivalent), 10% palladium on charcoal (0.1 equivalents) and ammonium formate (10 equivalents) in methanol was heated at reflux for 2 hours. The mixture was allowed to cool, filtered through Celite® and the filtrate concentrated in vacuo. The residue was partitioned between ethyl acetate and water, the organic phase washed with brine, dried (MgSO4), concentrated in vacuo and chromatographed on alumina, eluting with ethyl acetate, to give the desired compound as a colourless solid.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. temperatureto cool
4. filtrationfiltered through Celite®
5. concentrationthe filtrate concentrated in vacuo
6. customThe residue was partitioned between ethyl acetate and water
7. washthe organic phase washed with brine
8. dry with materialdried (MgSO4)
9. concentrationconcentrated in vacuo
10. customchromatographed on alumina
11. washeluting with ethyl acetate