Acetyl chloride → N-(2-Acetylphenyl)acetamide

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

ORDレコード

ord-28b2d8d4234a40a79511382c18032086

出典データセット

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09181264B2