関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | N-((Benzyloxy)carbonyl)-2-methylalanine | HCID 294936 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-[2-Benzyloxycarbonylamino-2-(methyl)propionylamino]ethanol | HCID 68947874 | — |
反応手順
To a solution of 2-benzyloxycarbonylamino-2-(methyl)propionic acid (1 g) in tetrahydrofuran (5 mL) was added 1,1′-carbonylbis-1H-imidazole (889 mg), and the mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 2-aminoethanol (0.38 mL), and the mixture was stirred at room temperature for 2 hours. The reaction mixture was purified by column chromatography on silica gel (eluent: dichloromethane/methanol=20/1) to give 2-[2-benzyloxycarbonylamino-2-(methyl)propionylamino]ethanol (973 mg). This material was dissolved in methanol (5 mL). To the solution was added 10% palladium-carbon powder (200 mg), and the mixture was stirred at room temperature under a hydrogen atmosphere overnight. The insoluble material was removed by filtration, and the solvent of the filtrate was removed under reduced pressure to give the title compound (505 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08324176B2 |
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| 出典データセット | uspto-grants-2012_12 |
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| ORD ID | ord-8c7dc730e87347978f022c1974e072e1 |
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| 出典メモ | uspto-grants-2012_12 |
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