関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexadecylamine | HCID 8926 | — |
| 反応物 | 2-Naphthalenesulfonyl chloride, 5-(acetylamino)-1-(acetyloxy)- | HCID 94125 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-Amino-2-hexadecylsulfamoyl-1-naphthol | HCID 20239903 | 54% |
反応手順
30 g of hexadecylamine was dissolved in 250 liters of acetone. To this solution was added gradually a solution of 40 g of 1-acetoxy-5-acetamino-naphthalene-2-sulfonyl chloride synthesized above in 150 ml of acetone while stirring, and, after completion of the addition, stirring was continued for about one hour at about 40° C. Then, the reaction solution was ice-cooled, and the precipitated crystals were collected by filtration and well washed with 1 liter of methanol. The crystals were refluxed for 8 hours together with 200 ml of ethanol, 30 g of NaOH, and 100 ml of water. After being allowed to cool to room temperature, the solution was neutralized with acetic acid, and the crystals thus precipitated were collected by filtration and recrystallized from an ethanol-water mixture solvent to obtain 22 g (54% yield) of product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04358532 |
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| 出典データセット | uspto-grants-1982_11 |
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| ORD ID | ord-025be907829a49caa92065a67490772f |
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| 出典メモ | uspto-grants-1982_11 |
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