関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 2-(2,4-dimethoxyphenyl)-N-methylacetamide | HCID 8180193 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(2-hydroxy-4-methoxyphenyl)-N-methylacetamide | HCID 69017352 | — |
| 生成物 | 2-(4-hydroxy-2-methoxyphenyl)-N-methylacetamide | HCID 69019532 | — |
反応手順
To a solution of 2-(2,4-dimethoxyphenyl)-N-methylacetamide (445 mg, 2.12 mmol) in CH2Cl2 (10 mL) was slowly added 1M BBr3 solution in CH2Cl2 (6.4 mL, 6.4 mmol). After addition was completed, the reaction mixture was stirred at 0° C. for 2.5 h, methanol (2 mL) was added and after 15 min the volatiles were removed in vacuo. The residue was dissolved in ethyl acetate, washed successively with aqueous NaHCO3 and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-5% methanol in dichloromethane) to give the subtitled compound (16 mg) along with 2-(4-hydroxy-2-methoxyphenyl)-N-methylacetamide (30 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07498338B2 |
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| 出典データセット | uspto-grants-2009_03 |
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| ORD ID | ord-4df6b0a2d19445ef82ebb5c8053a5c34 |
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| 出典メモ | uspto-grants-2009_03 |
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