関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Heptanone | HCID 8051 | — |
| 反応物 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 触媒 | Tetrabutylammonium Fluoride Trihydrate | HCID 11726816 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,1,1-Trifluoro-2-methyl-2-heptanol | HCID 80558715 | 102.3% |
反応手順
24.9 g of trimethyl(trifluoromethyl)silane, 16.0 g of 2-heptanone, 38 g of tetrahydrofuran and 350 mg of tetrabutylammonium fluoride trihydrate were charged into a four-necked flask equipped with a nitrogen feeding tube, a reflux condenser, a dropping funnel and a thermometer, and a reaction was effected by a conventional method. Then, 17.5 g of hydrochloric acid was dropwise added to the reaction mixture at a temperature of 25 to 48° C. over 30 minutes, followed by stirring at about 48° C. for 2 hours. The reaction mixture was treated by a conventional method, and the resulting organic phase was washed with a saline solution, followed by drying with anhydrous magnesium sulfate. Thereafter, the resultant was concentrated under reduced pressure, thereby obtaining 26.4 g of 1,1,1-trifluoro-2-methyl-2-heptanol in the form of a pale brown oily matter.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08105747B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-4b5604515fcc4a999830feb3f1db4cea |
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| 出典メモ | uspto-grants-2012_01 |
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