Triphenylphosphine → HCID 11557512, compound

Compound 46-2 (1.29 g) was dissolved in methylene chloride (30 ml), triphenylphosphine (2.62 g) and N-bromosuccinimide (1.76 g) were added under ice-cooling, and the mixture was stirred under ice-cooling for 2 hr. The reaction mixture was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether (50 ml) was added, and the precipitated triphenylphosphine oxide was filtered off. The concentrate of the filtrate was purified by silica gel column chromatography (hexane alone) to give the object product (760 mg) as a pale-yellow oil.

1. temperaturecooling
2. temperaturecooling for 2 hr
3. washThe reaction mixture was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. additionDiethyl ether (50 ml) was added
7. filtrationthe precipitated triphenylphosphine oxide was filtered off
8. concentrationThe concentrate of the filtrate
9. customwas purified by silica gel column chromatography (hexane alone)

ORD record

ord-ea824bcbc1ff4524bb581b61f0c9eab7

Source dataset

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08129361B2