関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Isobutyl chloride | HCID 10554 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | 3-Butyn-2-ol, 1,1,1-trifluoro-4-phenyl- | HCID 11412978 | — |
| 反応物 | HCID 178418368 | HCID 178418368 | — |
| 触媒 | Bis(cyclopentadienyl)titanium(IV) chloride | HCID 416358 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 20272630 | HCID 20272630 | 63% |
反応手順
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:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04532020 |
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| 出典データセット | uspto-grants-1985_07 |
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| ORD ID | ord-c7b863e996644d2aa218b8222f6844f3 |
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| 出典メモ | uspto-grants-1985_07 |
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