Benzyl Bromide → HCID 3473490, compound

Under nitrogen atmosphere, to a solution of ethyl magnesium chloride in tetrahydrofuran (1.58M, 95 ml) was added diethyl phosphite (6.91 g) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. To the mixture was added benzyl bromide (7.2 ml), and the mixture was refluxed for 4 hours. The reaction mixture was vigorously stirred and concentrated hydrochloric acid-ice was added to the mixture to stop the reaction. The mixture was extracted with diethylether and concentrated. To the residue was added chloroform, and the mixture was washed with water and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/ethanol=3:1→2:1) to give benzyldiethylphosphine oxide (1.45 g) as colorless crystals.

1. temperaturecooling
2. temperaturethe mixture was refluxed for 4 hours
3. stirringThe reaction mixture was vigorously stirred
4. customthe reaction
5. extractionThe mixture was extracted with diethylether
6. concentrationconcentrated
7. additionTo the residue was added chloroform
8. washthe mixture was washed with water
9. concentrationconcentrated under reduced pressure
10. customThe residue was separated
11. custompurified with column chromatography (ethyl acetate/ethanol=3:1→2:1)

ORD record

ord-55998afff1c84fcd9073ca67cf87bb06

Source dataset

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06268354B1