関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Phenylphosphonic Acid | HCID 15295 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 生成物 | HCID 21322899 | HCID 21322899 | — |
反応手順
The preparation was undertaken as a modification of the process for forming 3-carboxybenzenesulfonyl chloride as reported in J. Chem. Soc. (C), page 11 et seq. (1968) by R. J. W. Cremlyn. Phenylphosphonic acid was added in portions to chlorosulfonic acid; about 10 moles of chlorosulfonic acid per mole of phenylphosphonic acid were employed. The initial mixing step was exothermic, causing the temperature of the mixture to rise to about 90° C. After completion of the addition of the phenylphosphonic acid to the chlorosulfonic acid, the reaction mixture was heated to about 140° C. for about two hours. Reaction proceeded according to the equation ##STR5## Attempts to lower the molar ratio of chlorosulfonic acid: phenylphosphonic acid, by addition of sodium chloride (to remove sulfuric acid from the reaction mixture), caused uncontrollable frothing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04150021 |
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| 出典データセット | uspto-grants-1979_04 |
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| ORD ID | ord-2f67df89272540589f303ba72bc7384c |
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| 出典メモ | uspto-grants-1979_04 |
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