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-Chloro-5-methyl-3-nitropyridine | HCID 818300 | — |
| 反応物 | 4-Benzyloxyaniline hydrochloride | HCID 2723831 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 58577742 | HCID 58577742 | 22.8% |
反応手順
To a mixture of 4-(benzyloxy)aniline hydrochloride (4.10 g) and 2-chloro-5-methyl-3-nitropyridine (3.0 g) in DMF (30 mL) was added TEA (7.27 mL) at room temperature, and the mixture was stirred at room temperature for 2 h. The mixture was heated to 60° C. After stirring at 60° C. overnight, K2CO3 (4.81 g) was added to the mixture. The mixture was heated to 100° C. and stirred at 100° C. overnight. The mixture was poured into water and the mixture was extracted with AcOEt. The combined organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by column chromatography (dry charge, silica gel, eluted with 5%-30% AcOEt in hexane) to give N-[4-(benzyloxy)phenyl]-5-methyl-3-nitropyridin-2-amine (1.33 g) as a red solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846713B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-d89d58304d3c4849b30f48ebd5331560 |
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| 出典メモ | uspto-grants-2014_09 |
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