Potassium tert-butoxide → HCID 131729272, compound

Temperature

0 °C

Firstly, PPh3MeI (317 mg, 0.78 mmol: Me=methyl) was added with dist. toluene (4 mL). The resultant mixture was then added with KOt-Bu (88 mg, 0.78 mmol) at 0° C., and then was stirred under a nitrogen atmosphere at 0° C. for 30 minutes to obtain a mixture. Subsequently, the obtained mixture was added dropwise with a mixed solution (2 mL) of 4-(diallylethoxysilyl)benzaldehyde (204.2 mg, 0.78 mmol) obtained in Example 12 and dist. toluene under a nitrogen atmosphere at 0° C. The resultant mixture was stirred under a nitrogen atmosphere at 0° C. for 1.5 hours, and then was stirred at room temperature for 17 hours to obtain a reaction mixture. After that, a salt contained in the reaction mixture was removed through a celite filtration process. The organic layer thus obtained was then concentrated under reduced pressure to obtain a crude product. The obtained crude product was separated and purified by silica gel column chromatography (hexane/EtOAc=20/1) to obtain 4-(diallylethoxysilyl)styrene (134.3 mg, 66% yield).

1. additionFirstly, PPh3MeI (317 mg, 0.78 mmol: Me=methyl) was added with dist
2. customto obtain a mixture
3. customat 0° C
4. stirringwas stirred at room temperature for 17 hours
5. customto obtain a reaction mixture
6. customwas removed through a celite filtration process
7. customThe organic layer thus obtained
8. concentrationwas then concentrated under reduced pressure
9. customto obtain a crude product
10. customThe obtained crude product
11. customwas separated
12. custompurified by silica gel column chromatography (hexane/EtOAc=20/1)

ORD record

ord-c4b46053c88b459ea9346a072295234c

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08053588B2