関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Adamantanecarbonyl chloride | HCID 98915 | — |
| 反応物 | N-(N-Methylpiperidinyl)methylindole | HCID 11550392 | — |
| 反応物 | Diethyl aluminum chloride | HCID 16686102 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | AM-1248 | HCID 10293794 | — |
反応手順
To the stirring solution of the diethyl aluminum chloride (1.5 ml 1 M soln. in hexane, 180.8 mg, 1.5 mmol) in 10 ml absolute methylene chloride was added at room temp. 298.0 mg (1.5 mmol) 1-adamantanecarbonyl chloride in 5 ml of methylene chloride and the reaction mixture was stirred 15 min. The solution of (N-Methyl-2-piperidinyl)methyl-1H-indole (228.3 mg, 1.0 mmol) in 5 ml of methylene chloride was added during 3 min and mixture was stirred and reflux 48 h. The reaction was work-up by addition of 20 ml 2M solution of sodium hydroxide and extracted by ethyl acetate (3×20 ml), washed to times by water and two times by brine. The combined extract dried by the mixture of sodium sulfate and potassium carbonate. After removing of solvents the rest was purified by chromatography (silica gel, methanol ethyl acetate 1:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07173027B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-37550f74ddfb4842819c0a796d16908c |
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| 出典メモ | uspto-grants-2007_02 |
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