関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Bromo-2-butyne | HCID 2756862 | — |
| 反応物 | methyl 7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate | HCID 22328987 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate | HCID 22328992 | — |
反応手順
In THF (24.0 ml) was dissolved methyl 7-[4-(2-butoxyethoxy)phenyl]-2,3-dihydro-1-benzazepine-4-carboxylate (1.20 g). To the solution was added 60% sodium hydride (0.24 g), and the mixture was stirred at room temperature for 1 hour. To the mixture was added 1-bromo-2-butyne (0.80 ml), and the mixture was stirred at 65° C. for 4 days. After cooled to room temperature, the reaction solution was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate=4/1) to give methyl 7-[4-(2-butoxyethoxy)phenyl]-1-(2-butynyl)-2,3-dihydro-1-benzazepine-4-carboxylate (0.50 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06936602B1 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-74f01aa5068e4d44be7b05c6d1542084 |
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| 出典メモ | uspto-grants-2005_08 |
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