Potassium Phosphate, Tribasic → N-[3-(4-Ethyl-piperazin-1-yl)-phenyl]-N-methyl-acetamide

Temperature

100 °C

To a DMF solution (2.5 ml) of N-(3-bromo-phenyl)-N-methyl-acetamide (114 mg) obtained in Step B, palladium acetate (1.1 mg), S-Phos (4.1 mg) and potassium phosphate (212.3 mg), 1-ethylpiperazine (76.2 μl) was added, and then the mixture was degassed under ultrasonic irradiation. This was stirred at 100° C. for 5 hours, followed by addition of water (10 ml), which was extracted with ethyl acetate (10 ml×2), and the organic layer was dried over sodium sulfate. After the sodium sulfate was filtered off, the solvent was distilled off under reduced pressure, followed by purification by silica gel column chromatography (dichloromethane/methanol=20/1 to 10/1), to obtain the desired compound (104.9 mg, 80%).

1. customthe mixture was degassed under ultrasonic irradiation
2. additionfollowed by addition of water (10 ml), which
3. extractionwas extracted with ethyl acetate (10 ml×2)
4. dry with materialthe organic layer was dried over sodium sulfate
5. filtrationAfter the sodium sulfate was filtered off
6. distillationthe solvent was distilled off under reduced pressure
7. customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=20/1 to 10/1)

ORD record

ord-3329d1e0981640b48e87997bce9bcb6e

Source dataset

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08022205B2