Dimethylformamide → HCID 19350201, compound

A mixture of 2-(2-chloromethylphenyl)-2-oxoacetamide (3.41 g), potassium acetate (2.03 g), potassium iodide (0.14 g) and N,N-dimethylformamide (35 ml) was stirred at room temperature for 24 hours. To the reaction mixture was added a mixed solution (about 300 ml) of ethyl acetate and ether in a mixing ratio of about 1:1. The mixture was washed with water twice and saturated brine once. The resulting organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain the crude product (3.55 g). The crude product was recrystallized from ethyl acetate-hexane, the resulting mother liquor was concentrated under reduced pressure, and the residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:2) to give the title compound (2.62 g in total, yield: 68.6%, white crystals).

1. washThe mixture was washed with water twice
2. dry with materialThe resulting organic layer was dried over anhydrous sodium sulfate
3. customthe solvent was evaporated under reduced pressure
4. customto obtain the crude product (3.55 g)
5. customThe crude product was recrystallized from ethyl acetate-hexane
6. concentrationthe resulting mother liquor was concentrated under reduced pressure
7. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:2)

ORD record

ord-59520b2630af4c52a7c770f789c5b406

Source dataset

uspto-grants-2000_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06037495