Methanol → 1-Bromo-4-phenylbutane

To a solution of 4-phenyl-1-butanol (21.75 g) in acetonitrile (300 mL) was added triphenylphosphine dibromide (67.23 g) in portions with stirring over 10 min. After stirring over night under nitrogen, methanol (4 mL) was added and after 1.5 h, the solvent was removed under reduced pressure. Hexanes (200 mL) and ˜75 g silica gel were added to the residue and the mixture was filtered and the filter cake was eluted with hexanes. The clear filtrate was concentrated to give 32.8 g of clear colorless liquid. This product was again eluted through silica gel using 1.5 L hexanes to give the title compound (24.7 g) as a colorless liquid.

1. stirringAfter stirring over night under nitrogen
2. customthe solvent was removed under reduced pressure
3. additionHexanes (200 mL) and ˜75 g silica gel were added to the residue
4. filtrationthe mixture was filtered
5. washthe filter cake was eluted with hexanes
6. concentrationThe clear filtrate was concentrated

ORDレコード

ord-06693a3616814cb881bb4b289a4578b1

出典データセット

uspto-grants-2002_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06358979B1