Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Isobutyl chloride | HCID 10554 | — |
| Edukt | Magnesium | HCID 5462224 | — |
| Edukt | 3-Butyn-2-ol, 1,1,1-trifluoro-4-phenyl- | HCID 11412978 | — |
| Edukt | HCID 178418368 | HCID 178418368 | — |
| Katalysator | Bis(cyclopentadienyl)titanium(IV) chloride | HCID 416358 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | HCID 20272630 | HCID 20272630 | 63% |
Reaktionsschritte
In an isobutylmagnesium chloride solution that was prepared by reacting isobutyl chloride (3.74 g, 40 mmol) and magnesium (0.97 g, 40 mmol) in dry ether (40 ml) at 0° C., dichlorobis(π-cyclopentadienyl)titanium (0.22 g, 0.9 mmol) and 1,1,1-trifluoro-4-phenyl-3-butyne-2-ol (2 g, 10 mmol) were slowly added at 0° C. After 4 hour agitation of the mixture at room temperature, solvent was removed under heating for 30 min. Next, dry tetrahydrofuran (20 ml) was put into the reaction vessel and further methyl iodide (12.7 g, 90 mmol) was slowly added. After 12 hour agitation, the reaction mixture was treated by a method similar to the one in the above Examples to obtain (Z)-1,1,1-trifluoro-4-phenyl-3-pentene-2-ol (b.p.: 84°-86° C./2 mmHg) at a yield of 63%. The above product gave the following analytical data:
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04532020 |
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| Quelldatensatz | uspto-grants-1985_07 |
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| ORD ID | ord-c7b863e996644d2aa218b8222f6844f3 |
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| Quellennotiz | uspto-grants-1985_07 |
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