反应详情

To a 100-mL round-bottomed flask, phenyl(4-(trifluoromethyl)phenyl)-methanone (1.0105 g, 4.039 mmol) and methoxyamine (0.4208 g, 5.038 mmol) were dissolved in pyridine (10 mL). The mixture was stirred at rt overnight. Additional methoxyamine (0.1625 g) was added, and the solution was stirred at rt for 7 h. EtOAc was added and the organic phase was washed with water, 1 N HCl (2×), water, and then with brine. The organic phase was dried over sodium sulfate, filtered and concentrated in vacuo to afford a clear oil. The oil thus obtained was purified by Biotage (EtOAc/hexanes 0-20%) to afford the title compound (1.12 g, 99.4%) as a clear oil.

1. stirringthe solution was stirred at rt for 7 h
2. washthe organic phase was washed with water, 1 N HCl (2×), water
3. dry with materialThe organic phase was dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customto afford a clear oil
7. customThe oil thus obtained
8. customwas purified by Biotage (EtOAc/hexanes 0-20%)