反应详情

To a solution of (2-Acetylamino-4-chloro-phenyl)-acetic acid methyl ester )32.0 g, 133 mmol) in acetic acid (200 mL) stirred at 90 degree Celsius was added tert-butyl nitrite (20.5 mL, 172.3 mmol) over 1 hour. The reaction was poured into water (1.4 L) and the solids were recovered by filtration. The yellow precipitate was dissolved in EtOAc, then washed with saturated NaCl. The organic was dried over MgSO4, filtered, and concentrated to a solid. The solids were triturated with hexanes and filtered to afford the desired material (21.63 g, 77%).

1. filtrationthe solids were recovered by filtration
2. dissolutionThe yellow precipitate was dissolved in EtOAc
3. washwashed with saturated NaCl
4. dry with materialThe organic was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated to a solid
7. customThe solids were triturated with hexanes
8. filtrationfiltered