Hexane → (2-Bromomethylbenzyloxy)-t-butyldiphenylsilane

In dichloromethane (50 ml) were dissolved [2-[(t-butyldiphenylsilyloxy)methyl]phenyl]methanol (3.00 g, 7.97 mmol) and carbon tetrabromide (3.40 g, 10.3 mmol). Under ice cooling, a dichloromethane solution (5 ml) of triphenylphosphine (2.70 g, 10.3 mmol) was added dropwise. After stirring at room temperature for 14 hours, the reaction mixture was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel chromatography. The fraction obtained from the hexane:ethyl acetate=30:1 eluate was concentrated under reduced pressure, whereby the title compound (3.12 g, 7.10 mmol, 89%) was obtained as a colorless oil.

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. customThe residue thus obtained

ORD-Eintrag

ord-a4d8991de3e0447aaa3b2ac3885fc3c5

Quelldatensatz

uspto-grants-2008_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07399775B2