Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Carbon Dioxide | HCID 280 | — |
| Reactant | Triethoxychlorosilane | HCID 78398 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Reactant | 260262-38-2 | HCID 59710681 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Heptane | HCID 8900 | — |
| Product | HCID 59710676 | HCID 59710676 | 80% |
Reaction Steps
Magnesium (0.12 mol) and tetrahydrofuran were put in a 2-bulb flask purged with nitrogen. Then, 3-[(trifluorovinyl)oxy]bromobenzene prepared in (2) was dropped very slowly maintaining the reactor temperature at 0° C. The reactor was put in an ice bath to prevent the temperature from rising rapidly. After adding 3-[(trifluorovinyl)oxy]bromobenzene, the reactor was heated to room temperature, and reaction was performed for 2 hours. Then, triethoxychlorosilane (0.95 mol) was dropped keeping the reactor temperature at −48° C. with a constant temperature bath filled with dry ice and acetonitrile. The reaction mixture was mixed at room temperature for 24 hours. After the reaction was completed, excess heptane was added to remove the obtained salt and unreacted magnesium. The filtrate was removed by filtering with filter paper. Heptane remaining in the filtrate was removed using a vacuum evaporator and vacuum-distilled to obtain [3-[(trifluorovinyl)oxy]phenyl]triethoxysilane (PFCBSI) (yield: 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07368514B2 |
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| Source dataset | uspto-grants-2008_05 |
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| ORD ID | ord-0a7f19f08dc74087ac5562ff58253181 |
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| Source note | uspto-grants-2008_05 |
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