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Sulfuric Acid → 2-Chloro-6-fluoroaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2-Chloro-6-fluorobenzoic acid | HCID 67947 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Chloro-6-fluoroaniline | HCID 2734205 | — |
反応手順
To a stirred mixture of 20 g. of 2-chloro-6-fluorobenzoic acid, 100 ml. of chloroform and 50 ml. of concentrated sulfuric acid is added slowly 10.2 g. of sodium azide while the temperature is kept at 40°-55°. Stirring is continued for 2 hours at 40°-55° then the mixture is poured into 500 ml. of ice water containing 80 g. of sodium hydroxide. The mixture is extracted with ether and the other extracts are dried over magnesium sulfate. The dry extracts are then treated with hydrogen chloride, and the resultant product as the hydrochloride salt is collected by filtration yielding 12.6 g. of white solid which sublimes at 160°-170°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04032639 |
| 出典データセット | uspto-grants-1977_06 |
| ORD ID | ord-3e0bfc85cb5844a6a56847ee7894b893 |
| 出典メモ | uspto-grants-1977_06 |