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Water → HCID 23336373、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorobenzene | HCID 7964 | — |
| 反応物 | Diethylthiocarbamoyl chloride | HCID 66607 | — |
| 反応物 | 3-[N-(2,6-dimethylphenyl)carbamoyl]-4-methoxy-5-chloroaniline | HCID 23336374 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 23336373 | HCID 23336373 | 46% |
反応手順
A mixture of 3-[N-(2,6-dimethylphenyl)carbamoyl]-4-methoxy-5-chloroaniline (650 mg), diethylthiocarbamoyl chloride (360 mg) and chlorobenzene (6 ml) is refluxed for 30 minutes. The reaction mixture is mixed with water and shaken with methylene chloride. The organic layer is washed with water, dried over Glauber's salt and concentrated to remove the solvent. The residue is chromatographed on a column of silica gel, which is eluted with methylene chloride. The eluted fractions are collected and the solvent is evaporated. The residue is recrystallized from ethyl acetate to give 3-[N-(2,6-dimethylphenyl)carbamoyl]-4-methoxy-5-chlorophenyl isothiocyanate (340 mg) as crystals melting at 191°-192.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04228165 |
| 出典データセット | uspto-grants-1980_10 |
| ORD ID | ord-a3e6b58fc0954193b9c017c69ae5ecdc |
| 出典メモ | uspto-grants-1980_10 |