関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 2,4,5-Trichloronitrobenzene | HCID 6983 | — |
| 反応物 | 3-Amino-1-propanol | HCID 9086 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 3-((4,5-Dichloro-2-nitrophenyl)amino)-1-propanol | HCID 112955 | — |
反応手順
A mixture of 113.2 parts of 1,2,4-trichloro-5-nitrobenzene, 75 parts of 3-amino-1-propanol, 0.2 parts of potassium iodide and 200 parts of butanol is stirred and refluxed overnight. The butanol is removed by evaporation in vacuo and water is added to the residue. The product is extracted with 4-methyl-2-pentanone. The extract is washed a few times with water, dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The residue is triturated in 2,2'-oxybispropane. The product is filtered off and crystallized from a mixture of 2,2'-oxybispropane and 2-propanol, yielding 31.7 parts of 3-[(4,5-dichloro-2-nitrophenyl)amino]-1-propanol; mp. 97° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04175129 |
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| 出典データセット | uspto-grants-1979_11 |
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| ORD ID | ord-664c3c4a94474bb0a58d1ecfeccee38e |
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| 出典メモ | uspto-grants-1979_11 |
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