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Phosphorus oxychloride → 2-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | N-Methylformamide | HCID 31254 | — |
| 反応物 | 2-Naphthalenesulfonic acid, 5-(acetylamino)-1-(acetyloxy)-, sodium salt (1:1) | HCID 23663705 | — |
| 生成物 | 2-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)- | HCID 94125 | — |
反応手順
The 5-acetamido-1-acetoxynaphthalene-2-sulfonyl chloride was prepared by dropwise treatment of a suspension of dry sodium 5-acetamido-1-acetoxynaphthalene-2-sulfonate in 100 ml. phosphoryl chloride with 5.5 ml. dry methylformamide in a nitrogen atmosphere. The reaction mixture was stirred 1 hour and then poured over 600 ml. of crushed ice. The crude product was filtered and dissolved immediately in 500 ml. chloroform. The solution was treated with activated charcoal and dried over anhydrous magnesium sulfate to give 10.8 g. (44%) of a resinous yellow product which showed a single spot on a thin-layer chromotography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03954476 |
| 出典データセット | uspto-grants-1976_05 |
| ORD ID | ord-42c547f609ef49e793697d29c2f64f4a |
| 出典メモ | uspto-grants-1976_05 |