関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Azido-1-(3-methoxyphenyl)ethanone | HCID 18792863 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 2-Amino-1-(3-methoxyphenyl)ethanone | HCID 7176074 | 123.8% |
反応手順
Palladium on carbon (10 wt %, 10.41 g, 9.78 mmol) was added to a solution of 2-azido-1-[3-(methyloxy)phenyl]ethanone (1.87 g, 9.78 mmol) and hydrochloric acid (8.14 mL, 98 mmol) in CH3OH (50 mL) under nitrogen, and the reaction mixture was stirred under hydrogen overnight at 25° C. The mixture was filtered, washing with CH2Cl2 (50 mL) and CH3OH (100 mL), and then concentrated. Water (150 mL) was added, and the mixture was lyophilized to afford an HCl salt of the title compound (2.0 g) as a brown solid. LC-MS (ES) m/z=166 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08697685B2 |
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| 出典データセット | uspto-grants-2014_04 |
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| ORD ID | ord-ab9fdc775cf34e7b93852829c5416a1a |
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| 出典メモ | uspto-grants-2014_04 |
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