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2-Hydroxy-1-naphthaldehyde → 6-Bromo-2-hydroxy-1-naphthaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Hydroxy-1-naphthaldehyde | HCID 12819 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 6-Bromo-2-hydroxy-1-naphthaldehyde | HCID 735457 | 32.9% |
反応手順
To a solution of 2-hydroxy-1-naphthaldehyde (60.0 g) in AcOH (300 mL) was added dropwise a solution of bromine (66.8 g) in AcOH (30 mL) over 30 min. After being stirred for 1 h, the mixture was poured into aqueous Na2S2O3 solution, and the resulting mixture was extracted with AcOEt. The combined organic layers were washed with water, 1N-NaOH, and brine followed by drying over MgSO4. After removal of the solvent in vacuo, the residue was washed with EtOH to give a yellow powder. The powder was crystallized from iPrOH to afford the title compound (28.8 g) as pale yellow needles.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06649643B1 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-a87524f6e97d4e8f8078701930375b8b |
| 出典メモ | uspto-grants-2003_11 |