関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Fluoro-5-nitropyridine | HCID 95264 | — |
| 反応物 | tert-butyl N-((3-hydroxyphenyl)methyl)carbamate | HCID 18369568 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [3-(5-Nitro-pyridin-2-yloxy)-benzyl]-carbamic acid tert-butyl ester | HCID 68582589 | 43% |
反応手順
A mixture of (3-hydroxy-benzyl)-carbamic acid tert-butyl ester (250 mg, 1.12 mmol), 2-fluoro-5-nitro-pyridine (150 mg, 1.12 mmol) and K2CO3 (120 mg) in N,N-dimethylformamide (3 mL) was heated under microwave condition at 100° C. for 10 min. The reaction mixture was poured into water, and extracted with ethyl acetate (2×). The solvent was removed, and the resulting residue was chromatographered using hexane/ethyl acetate (7:1) to give the title compound (165 mg, 43%). MS (DCI/NH3) m/z 346 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07704997B1 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-c4fc933ec128489f9529b0d138d84950 |
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| 出典メモ | uspto-grants-2010_04 |
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