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Water → 2-chloro-N-(4-chlorobutyl-sulphonyl)-4-methyl-aniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Chloro-p-toluidine | HCID 12007 | — |
| 反応物 | 4-Chlorobutane-1-sulphonyl chloride | HCID 74212 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-chloro-N-(4-chlorobutyl-sulphonyl)-4-methyl-aniline | HCID 67048682 | — |
反応手順
1.30 ml (10.7 mmol) 2-chloro-4-methyl-aniline are placed in 30 ml of pyridine, combined with 2.67 g (10.5 mmol) 75% m 4-chlorobutyl-sulphonic acid chloride and stirred for 16 hours at ambient temperature. The reaction mixture is poured into water and extracted with ethyl acetate. The combined organic phases are washed with 6-molar hydrochloric acid, dried over sodium sulphate and evaporated down i. vac. The residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=9:1→7:3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07947700B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-4d703f5426c44af6b1c1cde516e6e502 |
| 出典メモ | uspto-grants-2011_05 |