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Dimethylformamide → 2-Hydroxy-4-morpholin-4-yl-benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-Morpholinophenol | HCID 141343 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Hydroxy-4-morpholin-4-yl-benzaldehyde | HCID 9815659 | 23% |
反応手順
DMF (10 mL) was treated dropwise with phosphorus oxychloride (2.3 g, 15 mmol). The reaction was kept at 25° C. by cooling on ice. The reaction mixture was treated with 3-(4-morpholinyl)phenol (2.5 g, 14 mmol) in small portions, stirred for 30 min at room temperature, then stirred at 100° C. for 8 h. After cooling, the mixture was poured into aqueous sodium acetate (1 M, 40 mL) and 10 mL of water was added. The resulting precipitate was collected by filtration, washed with water (10 mL), air dried, and purified by flash chromatography (silica gel, 4×7.5 cm, eluted with 90/10 CHCl3/ether) to yield the product as a light gray solid (0.66 g, 23%). See U.S. Pat. No. 4,147,552.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179912B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-0d94bf92443c410c9049b939710b8591 |
| 出典メモ | uspto-grants-2007_02 |