反应详情

To a white suspension of 1-(2-aminophenyl)ethanone (25 g, 185 mmol) and Et3N (33.4 mL, 240 mmol) in DCM at 0° C. was added dropwise AcCl (15.70 mL, 222 mmol) in 25 mL DCM. The reaction mixture was then stirred at r.t. for 2 h. After the reaction went to completion as monitored by LC-MS, the reaction mixture was cooled to 0° C., and was then quenched with H2O (100 mL). The organic phase was isolated; the aqueous layer was extracted with DCM. The organic phases were combined, and washed with H2O and brine. The resulting organic phase was dried over anhydrous MgSO4, filtered and concentrated to dryness to give crude N-(2-acetylphenyl)acetamide, which was used in the next step without further purification (30 g, yield 92%). MS (m/z): 136 (M+H)+.

1. temperaturethe reaction mixture was cooled to 0° C.
2. customwas then quenched with H2O (100 mL)
3. customThe organic phase was isolated
4. extractionthe aqueous layer was extracted with DCM
5. washwashed with H2O and brine
6. dry with materialThe resulting organic phase was dried over anhydrous MgSO4
7. filtrationfiltered
8. concentrationconcentrated to dryness