関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dibromomethane | HCID 3024 | — |
| 反応物 | 5-Bromo-3,4-dihydroxybenzaldehyde | HCID 85405 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Bromo-1,3-dioxaindane-5-carbaldehyde | HCID 2320243 | 60.5% |
反応手順
To a solution of 3-bromo-4,5-dihydroxy-benzaldehyde (1.52 g, 7.02 mmol) in DMF (20 mL), were added KF (4.077 g, 70.18 mmol) followed by dibromomethane (1 mL, 14.04 mmol) and the mixture heated at 140° C. for 4 hours. The solution was cooled to room temperature, water was added and the mixture extracted with ether. The organic layer was further washed with saturated aqueous NaHCO3, dried (MgSO4), filtered and evaporated to give 973 mg of 7-bromo-benzo[1,3]dioxole-5-carbaldehyde. 1H NMR (300 MHz; CDCl3): δ 6.16 (s, 2H), 7.26 (s, 1H), 7.54 (s, 1H), 9.76
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07196108B2 |
|---|
| 出典データセット | uspto-grants-2007_03 |
|---|
| ORD ID | ord-0d38999cde49444faa0534a1045bfd1b |
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| 出典メモ | uspto-grants-2007_03 |
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