関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Bromosalicylaldehyde | HCID 72863 | — |
| 反応物 | Methyl 3-(p-tolylsulfonyloxy)-2,2-dimethylpropanoate | HCID 22479327 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Bromo-2-formyl-phenoxy)-2,2-dimethyl-propionic acid methyl ester | HCID 57565919 | 85.7% |
反応手順
To a mixture of 5-bromo-2-hydroxy-benzaldehyde (4 g, 20 mmol), KI (1 g) and K2CO3 (4 g, 29 mmol) in DMF (10 mL) was added 2,2-dimethyl-3-(toluene-4-sulfonyloxy)-propionic acid methyl ester (6.9 g, 24 mmol). The mixture was heated at 140° C. for 2 h, and then cooled to room temperature, partitioned between water and ethyl acetate. The organic layer was washed with water (3×), dried over anhydrous Na2SO4 and concentrated. The residue was purified by column chromatography to give the title compound (5.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08134001B2 |
|---|
| 出典データセット | uspto-grants-2012_03 |
|---|
| ORD ID | ord-fba2758d098a4d34b42fece0f2cc4f18 |
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| 出典メモ | uspto-grants-2012_03 |
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