関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Methoxy-o-toluidine | HCID 99500 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 5-Methoxy-2-methylphenol | HCID 10953582 | — |
反応手順
To a solution of 2-methyl-5-(methyloxy)aniline (Intermediate 11, 6.0 g) in H2SO4 (5 M, 20 mL) was added portionwise NaNO2 (3.4 g, 49.3 mmol) at 0-5° C. The mixture was stirred at 50° C. for 1 hour and extracted with ethyl acetate (4 times 30 mL). The combined ethyl acetate layers were dried over sodium sulphate and concentrated under vacuum to give a residue, which was purified by column chromatography on silica gel (with EtOAc:PE=1:20 as eluents) to afford the title compound as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08722695B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-fc2fd5de506447e79b94c5ac31b799aa |
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| 出典メモ | uspto-grants-2014_05 |
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