関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Sodium Tartrate | HCID 9357 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 1-Acetyl-1-(3,4-dichlorophenyl)cyclobutane oxime | HCID 86031113 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-[1-(3,4-Dichlorophenyl)cyclobutyl]ethylamine | HCID 13083140 | — |
反応手順
A solution of the oxime prepared above (4.0 g) in ether (50 ml) was added slowly to a stirred suspension of lithium aluminium hydride (0.9 g) in ether (50 ml) under nitrogen. The mixture was heated under reflux for one hour and, after cooling, water and then a 20% aqueous solution of Rochelle's salt (potassium sodium tartrate tetrahydrate) (27 ml) and a 10% aqueous solution of sodium hydroxide (6 ml) added. The reaction mixture was stirred for one hour and then continuously extracted with ether during eighteen hours. The ether extract was dried and the ether removed to leave a solid from which 1-[1-(3,4-dichlorophenyl)cyclobutyl]ethylamine was separated by high pressure liquid chromatography. The product was identified by standard analytical techniques as the compound of Example 1 in the form of its free base.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04767790 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-f58e48150f6d4f5bacb8a34d603b8129 |
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| 出典メモ | uspto-grants-1988_08 |
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