関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Boron Trichloride | HCID 25135 | — |
| 反応物 | 1,4-Dimethoxy-2-methyl-5-nitrobenzene | HCID 2778095 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methoxy-5-methyl-2-nitrophenol | HCID 57418664 | 99.6% |
反応手順
1-Methyl-2,5-bis(methyloxy)-4-nitrobenzene (3.96 g, 20 mmol) was dissolved in CH2Cl2 (20 mL) and cooled to −20° C. A solution of BCl3 (1.0 M) in CH2Cl2 (20 mL) was added to above solution drop wise over 5 minutes. A purple solution was obtained. The reaction mixture was slowly warmed to room temperature and stirred for 20 h. The mixture was then quenched with saturated Na2CO3, stirred for 10 minutes and then extracted with EtOAc (3×100 mL). The organic extracts were combined, washed with water, brine, and dried (Na2SO4). The solvent was removed via rotovap to give the title compound (3.65 g, 99%) as a yellow solid. MS (ES) m/e 184 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07432258B2 |
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| 出典データセット | uspto-grants-2008_10 |
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| ORD ID | ord-edd55955f8b643e99ea96a7bbb044fd8 |
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| 出典メモ | uspto-grants-2008_10 |
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