1,1-Dibromoethane → HCID 57659389, compound

To a slurry of magnesium (2.43 g) in dry tetrahydrofuran (50 mL), few drops of dibromoethane (˜50 μL) was added under argon and stirred at room temperature for 10 min. The reaction mixture was cooled to 10° C. and 2-(2-bromoethyl)-1,3-dioxolane (10.9 g) was introduced dropwise during 10 min and allowed to stir at room temperature for 2 hours. The resulting reaction mixture was cooled to −10° C. and allyldimethylchlorosilane (6.73 g) was added dropwise during 10 min. and stirred over night at room temperature. Finally, the reaction content was quenched with aqueous NaHCO3 (15 mL) and extracted with ether (3×50 mL). The combined organic layer was dried and concentrated under mild vacuum to obtain the crude product, which was advanced to the next step without further purification (yield 9.5 g).

1. temperatureThe reaction mixture was cooled to 10° C.
2. stirringto stir at room temperature for 2 hours
3. customThe resulting reaction mixture
4. temperaturewas cooled to −10° C.
5. stirringstirred over night at room temperature
6. customFinally, the reaction content was quenched with aqueous NaHCO3 (15 mL)
7. extractionextracted with ether (3×50 mL)
8. customThe combined organic layer was dried
9. concentrationconcentrated under mild vacuum

ORD record

ord-7394fa015b1347c9a15e28d54897c96a

Source dataset

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07687496B2