Chlorotrimethylsilane → HCID 178505823, compound

Temperature

150 °C

Zinc powder (2.62 g, 40.00 mmol) and lithium chloride (1.696 g, 40.00 mmol) were added to a dried flask and heated to 150° C. under vacuum for 30 min. The flask was allowed to reach room temperature. THF (20 mL) and 1,2-dibromoethane (0.115 mL, 1.33 mmol) were added. The mixture was heated until boiling occurred and the flask was then allowed to reach room temperature. Chlorotrimethylsilane (0.034 mL, 0.27 mmol) was added and the mixture was again heated until boiling occurred. The flask was cooled with an ice-bath and 5-(bromomethyl)-1,2,3-trifluorobenzene (6 g, 26.67 mmol) dissolved in THF (5 mL) was then added dropwise. The ice-bath was removed and the reaction stirred at room temperature for 20 h. Solids were allowed to settle and the supernatant used in the next transformation.

1. customto reach room temperature
2. temperatureThe mixture was heated
3. customto reach room temperature
4. temperaturethe mixture was again heated
5. temperatureThe flask was cooled with an ice-bath
6. additionwas then added dropwise
7. customThe ice-bath was removed

ORD record

ord-d8fa14aa9e404e519b83680924685a75

Source dataset

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08415378B2