化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-Amino-4-methoxy-benzenesulfonic acid 3,4,5-trimethoxy-phenyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3,4,5-Trimethoxyphenol | HCID 69505 | — |
| 反応物 | 3-Amino-4-methoxyphenylsulphonyl fluoride | HCID 96952 | — |
| 反応物 | t-Butylammonium Iodide | HCID 22344722 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Amino-4-methoxy-benzenesulfonic acid 3,4,5-trimethoxy-phenyl ester | HCID 9820655 | 35% |
反応手順
A solution of 3,4,5-trimethoxyphenol (505.7 mg, 2.75 mmol) in dichloromethane (28 mL) was treated sequentially with triethylamine (1.2 mL), 4-methoxymetanilyl fluoride (572.5 mg, 2.75 mmol), and tert-butylammonium iodide (106 mg, 0.287 mmol), stirred overnight, and washed once with 1M Na2CO3. The organic layer was separated, dried (MgSO4), filtered, and concentrated. Chromatography of the concentrate on silica gel with 40% ethyl acetate/hexanes provided 356 mg of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06521658B1 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-3462e9bbd0674957b0e4a1b6e9cb8fd0 |
| 出典メモ | uspto-grants-2003_02 |