Chlorotrimethylsilane → HCID 178505820, compound

Temperature

60 °C

In a dried flask was zinc powder (3.05 g, 46.69 mmol) suspended in anhydrous tetrahydrofuran (25 mL) under nitrogen. The resulting suspension was warmed to 60° C., then 1,2-dibromoethane (0.168 mL, 1.95 mmol) was added and stirred at that temperature for 15 min. It was cooled to room temperature, then chlorotrimethylsilane (0.2 mL, 1.58 mmol) was added and stirred at room temperature for 1 h 15 min. Then, 4-(bromomethyl)-2-fluoro-1-(trifluoromethyl)benzene (10 g, 38.91 mmol) in tetrahydrofuran (5 mL) was added in 6 equal portions every 10 minutes under ice-cooling. After complete addition the ice-bath was removed and the reaction mixture stirred at room temperature for 18 h. Then was stirring switched off to let the solids settle. The supernatant was used in next transformation.

1. customIn a dried flask was
2. temperatureIt was cooled to room temperature
3. stirringstirred at room temperature for 1 h 15 min
4. temperaturecooling
5. customwas removed
6. stirringthe reaction mixture stirred at room temperature for 18 h
7. stirringThen was stirring

ORD record

ord-d70ef8bc7cb5400a9cc604d80f59db14

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08415378B2