関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Nitropropane | HCID 398 | — |
| 反応物 | Ethanol, 1-ethoxy-2,2,2-trifluoro- | HCID 9897 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Methyl-3-nitro-1,1,1-trifluorobutan-2-ol | HCID 19936542 | — |
反応手順
A mixture of triflouroacetaldehyde ethyl hemiacetal (2.58 ml), 2-nitropropane (1.81 ml) and potassium carbonate (111 mg) is stirred at 65° C. (oil bath temperature) for 6 hours followed by 2.5 days at room temperature. The reaction mixture is diluted with water (100 ml) and extracted with methylene chloride (100 ml+5×50 ml). The combined organic layers are dried over sodium sulphate and the solvent is evaporated under reduced pressure. Purification of the liquid residue by flash chromatography on silica gel (eluant n-hexane/ethylacetate 85:15) affords 3-methyl-3-nitro-1,1,1-trifluorobutan-2-ol as an oil (2.005 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05418238 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-dd1d05ae442b432398f97755dff0385d |
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| 出典メモ | uspto-grants-1995_05 |
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