Carbon Tetrachloride → HCID 66607261, Verbindung

Temperatur

80 °C

A mixture of N′-[(3,4-difluorophenyl)acetyl]-3-methoxy-4-(2-methyl-1,3-oxazol-5-yl)benzohydrazide (4.69 g), carbon tetrachloride (2.24 mL) and triphenylphosphine (12.3 g) in acetonitrile (117 mL) was stirred at 80° C. for 2 hr. The mixture was allowed to cool to room temperature, the precipitate was filtered off, and the filtrate was concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate). Ethyl acetate was added to the obtained crude product, the precipitate was filtered off, and the filtrate was concentrated. Acetonitrile was added to the obtained residue, and the resultant precipitate was collected by filtration to give the title compound (2.41 g).

1. temperatureto cool to room temperature
2. filtrationthe precipitate was filtered off
3. concentrationthe filtrate was concentrated
4. additionWater was added to the residue
5. extractionthe mixture was extracted with ethyl acetate
6. dry with materialThe extract was dried over anhydrous magnesium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (ethyl acetate)
9. additionEthyl acetate was added to the
10. customobtained crude product
11. filtrationthe precipitate was filtered off
12. concentrationthe filtrate was concentrated
13. additionAcetonitrile was added to the obtained residue
14. filtrationthe resultant precipitate was collected by filtration

ORD-Eintrag

ord-0320ab33daf247e486533b44fd9b5b00

Quelldatensatz

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08901309B2