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Hydrochloric Acid → 2,6-Dimethylbenzylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | N-(2,6-Dimethylbenzyl)phthalimide | HCID 10825581 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2,6-Dimethylbenzylamine | HCID 12622912 | — |
反応手順
To a stirred solution of N-(2,6-Dimethylbenzyl)phthalimide (Step B, 7.77 g, 29.3 mmol) in ethanol (80 ml) was added hydrazine monohydrate (2.16 ml, 44.52 mmol) and the reaction mixture was refluxed for 3.5 hours. To this reaction mixture was added c HCl to bring pH to 1 and refluxing continued for another 3.5 hours, water was added and reaction mixture was filtered, the filtrate was concentrated and pH was adjusted to 10 with 2 N NaOH. The residue was taken in methylene chloride and washed with brine, dried over Na2SO4, filtered and concentrated to give an oil which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06946491B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-12b6f75028544381a30f4f437c61b54e |
| 出典メモ | uspto-grants-2005_09 |