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Sodium Bicarbonate → 4-Methoxy-2-nitrobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-(Dibromomethyl)-4-methoxy-2-nitrobenzene | HCID 3502335 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Methoxy-2-nitrobenzaldehyde | HCID 357691 | 85% |
反応手順
A mixture of 1-(dibromomethyl)-4-methoxy-2-nitrobenzene (42 g, 0.23 mol) and NaHCO3 (3 Eq) in water (400 mL) is refluxed for 22 h. The reaction mixture is cooled to room temperature and the product is extracted with EtOAc (2×150 mL). The organic layer is washed with a solution of 1.5N HCl (2×100 mL), water (2×100 mL) and brine then dried over Na2SO4. The solvent is removed under reduced pressure to afford 20 g (85%) of the title compound as a brown solid. 1H NMR (DMSO-d6, 400 MHz) δ 10.03 (s, 1H), 7.93-7.95 (m, 1H), 7.61 (s, 1H), 7.40-7.41 (m, 1H), 3.93 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08614215B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-810510ceaf56408aadd3a32e6869fdf2 |
| 出典メモ | uspto-grants-2013_12 |