関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | [3-(Bromomethyl)oxetan-3-yl]methanol | HCID 529264 | — |
| 反応物 | 2-Chloro-4-(trifluoromethyl)phenol | HCID 2736603 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | [3-(2-Chloro-4-trifluoromethylphenoxymethyl)oxetan-3-yl]-methanol | HCID 58031838 | — |
反応手順
600 mg of 3-chloro-4-hydroxybenzotrifluoride and 829 mg of 3-bromomethyl-3-oxetanemethanol were dissolved in 20 ml of acetonitrile, and 1.49 g of cesium carbonate were added. The reaction mixture was heated to 110° C. and stirred at this temperature for three hours. 50 ml of water and 50 ml of ethyl acetate were added to the cooled reaction mixture. The organic phase was removed, dried over MgSO4 and then concentrated under reduced pressure. The residue was purified on silica gel with the n-heptane/ethyl acetate solvent mixture as a linear gradient of 100% n-heptane=>100% ethyl acetate. This gave 990 mg of [3-(2-chloro-4-trifluoromethylphenoxymethyl)oxetan-3-yl]methanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08859494B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-ee84e78adf8f46ed9d0860a704466fc9 |
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| 出典メモ | uspto-grants-2014_10 |
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