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Thionyl Chloride → HCID 13105626、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3-((4,5-Dichloro-2-nitrophenyl)amino)-1-propanol | HCID 112955 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 13105626 | HCID 13105626 | — |
反応手順
To a stirred mixture of 10 parts of 3-[(4,5-dichloro-2-nitrophenyl)amino]-1-propanol and 75 parts of trichloromethane are added dropwise 11.2 parts of sulfinyl chloride. Upon completion, stirring is continued for 4 hours at reflux temperature. The reaction mixture is evaporated and the residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 4,5-dichloro-N-(3-chloropropyl)-2-nitrobenzenamine; mp. 78° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04377578 |
| 出典データセット | uspto-grants-1983_03 |
| ORD ID | ord-21b05452eba24d8784dfac9975561586 |
| 出典メモ | uspto-grants-1983_03 |