Chlorotrimethylsilane → HCID 68962089, compound

Temperature

2.5 °C

21.3 g (100 mmol) of 2-allyl-4-bromophenol, 12.1 g (120 mmol) of triethylamine (hereinafter referred to as “TEA”), and 120 ml of distilled tetra hydrofuran (hereinafter referred to as “THF”) were loaded into a 300-ml four-necked flask equipped with a reflux pipe with a calcium chloride dry pipe, a dropping funnel, a nitrogen gas introducing pipe, and a mechanical stirring device. The mixture was placed under nitrogen, and was stirred at 0 to 5° C. During the stirring, 11.0 g (120 mmol) of chlorotrimethylsilane were slowly added to the mixture from the dropping funnel. After the completion of the dropping, the resultant was subjected to a reaction at the temperature for 1 hour and then at room temperature for 6 hours. After that, the solvent, excessive trimethylamine, and excessive chlorotrimethylsilane were removed by condensation under reduced pressure, and the residue was washed with water and dried. Thus, 2-allyl-4-bromo-1-trimethylsiloxybenzene was quantitatively obtained.

1. customwere loaded into a 300-ml four-necked flask
2. customdry pipe, a dropping funnel
3. additiona nitrogen gas introducing pipe
4. customAfter the completion of the dropping, the resultant was subjected to a reaction at the temperature for 1 hour
5. customAfter that, the solvent, excessive trimethylamine, and excessive chlorotrimethylsilane were removed by condensation under reduced pressure
6. washthe residue was washed with water
7. customdried

ORD record

ord-72d5f662113d40f6aab63b5e9bb3373b

Source dataset

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07557152B2