関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Azabicyclo(2.2.2)octan-3-one | HCID 137887 | — |
| 反応物 | 2-Chloro-6,7-dimethoxyquinoxaline | HCID 22573137 | — |
| 溶媒 | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| 生成物 | 2-(6,7-Dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-one | HCID 22573161 | 34.9% |
反応手順
2-Azabicyclo[2.2.2]octan-3-one (228 mg, 2.3 mmole) is dissolved in a mixture of THF/DMF (5 mL/3 mL) and treated with NaH (60%, 184 mg, 4.6 mmole). The resulting mixture is heated at 60° C. for 0.5 hour before addition of 2-chloro-6,7-dimethoxyquinoxaline (344 mg, 1.5 mmole). After being heated at 80° C. overnight, the reaction mixture is concentrated . The residue is chromatographed on silica gel (50% ethyl acetate/hexane) to give 164 mg (23%) of a yellow solid (m.p. 158-159° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06180632B2 |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-c5946580d86643d89c693cc7815d6d15 |
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| 出典メモ | uspto-grants-2001_01 |
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