関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1(2H)-Phthalazinone | HCID 8394 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(2-Bromoethoxy)benzaldehyde | HCID 2735565 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-[2-[1-oxo-2(1H)-phthalazinyl]ethoxy]benzaldehyde | HCID 86760424 | 90% |
反応手順
A mixture of 3-(2-bromoethoxy)benzaldehyde (6.00 g), 1(2H)-phthalazinone (4.21 g), potassium carbonate (7.24 g) and N,N-dimethylformamide (40 ml) was stirred at 80° C. for 5 hours. After cooling, the reaction mixture was poured into water, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4) and concentrated to obtain 3-[2-[1-oxo-2(1H)-phthalazinyl]ethoxy]benzaldehyde (6.94 g, yield 90%) as colorless crystals. This was recrystallized from acetone-hexane. Melting point: 110–111° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07179823B1 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-52c13e04fc4342d2a5bbbbb521c99b09 |
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| 出典メモ | uspto-grants-2007_02 |
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