Allyl bromide → HCID 67197848, compound

Temperature

-78 °C

A 1.9 M tetramethyldisilazane sodium-tetrahydrofuran solution (9.44 mL, 18.0 mmol) was added dropwise over 10 minutes to a tetrahydrofuran (40 mL) solution of ethyl 2-cyclobutylacetate (2.32 g, 16.3 mmol) cooled to −78° C., and the mixture was then stirred at −78° C. for 10 minutes. Subsequently, a tetrahydrofuran (10 mL) solution of allyl bromide (7.90 g, 65.3 mmol) was added dropwise thereto over 10 minutes, and the mixture was stirred at room temperature for 17 hours. The mixture was treated with water, and volatile portions were then removed under reduced pressure. To the obtained liquid, ethyl acetate and water were added, and the obtained organic layer was dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure to obtain the compound of interest as a yellow oil substance (1.80 g, 61%).

1. waitover 10 minutes
2. stirringthe mixture was stirred at room temperature for 17 hours
3. customwere then removed under reduced pressure
4. additionTo the obtained liquid, ethyl acetate and water were added
5. dry with materialthe obtained organic layer was dried over anhydrous magnesium sulfate
6. distillationThen, the solvent was distilled off under reduced pressure
7. customto obtain the compound of interest as a yellow oil substance (1.80 g, 61%)

ORD record

ord-99f6bc43bbdd4fb7b54f431eac15f295

Source dataset

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07947738B2