関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 1,4-Dibromo-2-chloro-1,1,2-trifluorobutane | HCID 136221 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Bromo-3-chloro-3,4,4-trifluorobutan-1-ol | HCID 21836477 | 49% |
反応手順
A mixture of 1,4-dibromo-2-chloro-1,1,2-trifluorobutane (XVI) (7.5 g, 24.6 mmol), 1-methyl-2-pyrrolidinone (14 mL) and water (2.5 mL) was heated at 130° C. for 16 hours. The mixture was cooled to room temperature, diluted with water (80 mL) and extracted with ether (2×75 mL). The ether extract was washed with water (31×40 mL), brine, and dried over anhydrous magnesium sulfate. The residue obtained after evaporation of the solvent was chromatographed over silica gel to give 2.9 g (49%) of the desired alcohol as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05514717 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-d50b6a50e67449de839290b11556f0b4 |
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| 出典メモ | uspto-grants-1996_05 |
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