関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Decane | HCID 15600 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | 2-(2-Chloroethoxy)benzene-1-sulfonamide | HCID 13729454 | — |
反応手順
A process according to claim 1, wherein the compound of formula II is reacted with ethylene carbonate in the presence of a catalytic amount of tributylamine at a temperature between +130° C. and +150° C.; the resulting reaction mixture is treated with phosgene in the presence of a catalytic amount of dimethylformamide at a temperature between +70° C. and +90° C. yielding the compound of formula IV, which after purification is treated with 1 equivalent of chlorosulfonic acid or with a slight excess thereof in cyclohexane or n-decane at a temperature between +20° C. and +60° C.; neutralized with aqueous sodium hydroxide at a temperature between +50° C. and +90° C.; dechlorinated with hydrogen in the presence of an acid acceptor, in the pressure range from 1 to 5 bar at a temperature between +20° C. and +70° C. and in the presence of a 5% palladium on carbon catalyst; converted to the sulfonic acid chloride by treatment of the mixture with phosgene at a temperature between +60° C. and +120° C.; and subsequently reacted to the final product by treatment of the reaction mixture with an aqueous solution of ammonia.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04806528 |
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| 出典データセット | uspto-grants-1989_02 |
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| ORD ID | ord-dba526094804483395f13c80f0fc0217 |
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| 出典メモ | uspto-grants-1989_02 |
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