関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4-Nitroaniline | HCID 7475 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,1'-(Phenylimino)bis[3-chloro-2-propanol] | HCID 13479414 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(N,N-Diglycidylamino)-4'-nitroazobenzene | HCID 21700519 | 34% |
反応手順
0.25 mol of 4-nitroaniline are stirred in 150 ml of 16% aqueous hydrochloric acid and diazotized at 0° to 5° C. with 0.25 mol of sodium nitrite in 100 ml of water. The diazonium salt solution is filtered, added drop by drop to a solution of 0.25 mol N,N-bis(3-chloro-2-hydroxypropyl)-aniline in 250 ml 5% aqueous hydrochloric acid at 5° to 10° C. and stirred 1 h. The suspension obtained is neutralized with 25% aqueous ammonia solution, 1000 ml of 50% aqueous caustic soda solution are then added drop by drop and stirring takes place for 1 h. The precipitate is drawn off and washed until neutral. The crude product is then dried and chromatographed on silica gel with dichloromethane/tetrahydrofuran as elution agent (yield: 34%); MP: 135°-136° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420172 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-bdae0a84e29d461fb55eb7698802efc4 |
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| 出典メモ | uspto-grants-1995_05 |
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