Acetic Anhydride → HCID 73031688, compound

In 10 ml of dimethylacetamide was dissolved 0.84 g (1.8 mmol) of 3-(3-pyridylmethylideneamino)-3,4-dihydro-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, and to the resulting solution was added 0.09 g (2.3 mmol) of sodium hydride (purity: 62.4%). The reaction was carried out at room temperature for 30 minutes, after which 0.25 g (2.4 mmol) of acetic anhydride was added and the reaction was carried out for 4 hours. After completion of the reaction, the reaction solution was poured into ice water and the desired compound was extracted with ethyl acetate (20 ml×3). The extract solution was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated in vacuo. The crude product thus obtained was purified by silica gel column chromatography (ethyl acetate−methanol=10:1) to obtain 0.78 g of the desired compound.

1. waitthe reaction was carried out for 4 hours
2. customAfter completion of the reaction
3. extractionthe desired compound was extracted with ethyl acetate (20 ml×3)
4. washThe extract solution was washed with water and saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude product thus obtained
8. customwas purified by silica gel column chromatography (ethyl acetate−methanol=10:1)

ORD record

ord-ec75481853414e9c95bd9ae8da094b36

Source dataset

uspto-grants-2011_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08034931B2