関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Dibromobutane | HCID 8056 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 反応物 | Methyl 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropionate | HCID 9877912 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[1-Hydroxy-2,2,2-trifluoro-1-(trifluoromethyl)ethyl]cyclopentanol | HCID 58939317 | 89% |
反応手順
A flask was charged with 9.7 g of magnesium and 200 ml of tetrahydrofuran, to which 43.2 g of 1,4-dibromobutane was added dropwise at 60° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 22.4 g of the target compound (yield 89%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07868199B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-b31391d3bffb4b50a3e35a23f49ffb54 |
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| 出典メモ | uspto-grants-2011_01 |
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