Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-Propene, 2-bromo-3,3,3-trifluoro- | HCID 272696 | — |
| Reactant | (2,2,3,3,4,4,5,5-Octafluoropentyl)propanedinitrile | HCID 25242027 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Product | HCID 86612546 | HCID 86612546 | 0.9% |
Reaction Steps
1.4 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile was dissolved in 6 ml of a solution (1 mol/L) of tetrabutylammonium fluoride in tetrahydrofuran and then cooled to 0° C. Thereto 1.1 g of 2-bromo-3,3,3-trifluoropropene dissolved in 3 ml of tetrahydrofuran was added dropwise, and the mixture was stirred at room temperature for 8 hours and at 60° C. for 5 hours. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with methyl tert-butyl ether. The organic layer was washed successively with water, aqueous saturated sodium hydrogen carbonate and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.02 g of 2-(2,2,3,3,4,4,5,5-octafluoropentyl)-2-(2-bromo-3,3,3-trifluoropropyl)malononitrile (hereinafter, referred to as the present compound (57)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07662402B2 |
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| Source dataset | uspto-grants-2010_02 |
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| ORD ID | ord-b3dc812194434a08817c045cd7bbecbc |
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| Source note | uspto-grants-2010_02 |
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