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Veratrole → 3,4-Dimethoxybenzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Veratrole | HCID 7043 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Bis(3,4-dimethoxyphenyl)methanone | HCID 223042 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | 3,4-Dimethoxybenzophenone | HCID 286742 | — |
反応手順
3,4-Dimethoxybenzophenone was prepared analogously to 3,4,3',4'-tetramethoxybenzophenone using veratrole (2 mL, 15 mmol), aluminum chloride (2.2 g, 16.5 mmol) and benzoyl chloride (1.8 mL, 15.5 mmol). The crude mixture was purified by flash column chromatography (silica gel, 3% ethyl acetate/methylene chloride) to yield 3.44 g (93%) of the product as a white solid: mp 99-100° C.; 1H NMR (CDCl3) δ 7.82-7.30(m, 7H), 6.95-6.85 (m, 1H), 3.96 (s, 3H), 3.94 (s, 3H); 13C NMR (CDCl3) δ 195.5, 153.0, 149.0, 138.2, 131.8, 130.2, 129.6, 128.1, 125.4, 112.1, 109.7, 56.0, 56.0; Anal. Calcd for C15H14O3. Theoretical: C, 74.36; H, 5.82. Found: C, 74.21; H, 6.01.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05929117 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-d42586159a8841cca8f416680f3f499c |
| 出典メモ | uspto-grants-1999_07 |