関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1,3,4,5-Tetrahydro-2H-1-benzazepin-2-one | HCID 248580 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | Methyl 4-(2-aminophenyl)butanoate | HCID 237256 | — |
反応手順
To 1,3,4,5-tetrahydro-benzo[b]azepin-2-one (1 g, 6.2 mmol) in MeOH (8 mL), concentrated sulfuric acid (0.5 mL) was added and the mixture was stirred at room temperature for 2 hrs and at 70° C. for an additional hr. The solvent was removed and DCM and water were added. The organic layer was removed and the aqueous layer was basified with sat NaHCO3 and extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo to yield 4-(2-amino-phenyl)-butyric acid methyl ester (0.93 g). MS [M+H]+: 194.1; tR=1.49 min. (method 1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08084614B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-5c29b101b31d4bca86da92c6731414c6 |
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| 出典メモ | uspto-grants-2011_12 |
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