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Chlorosulfonic acid → 4-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | 3-Methoxy-1,2,4,5-tetramethylbenzene | HCID 278664 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methoxy-2,3,5,6-tetramethylbenzenesulfonyl chloride | HCID 15917520 | — |
反応手順
In 600 ml of dichloromethane was dissolved 10.0 g of 2,3,5,6-tetramethylanisole, followed by addition of a solution (400 ml) of 12 ml of chlorosulfonic acid in dichloromethane at -5°~-10° C. The mixture was kept stirred for 2 hours and the reaction mixture was poured into ice-5% aqueous NaHCO3. The organic layer was washed with water and dried over magnesium sulfate. The solvent was distilled off and the residue was crystallized from n-hexane and filtered.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04487726 |
| 出典データセット | uspto-grants-1984_12 |
| ORD ID | ord-c254c37c89bf40f29c916ef78cc2ef2d |
| 出典メモ | uspto-grants-1984_12 |