関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Salicylaldehyde | HCID 6998 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Chloro-4,6-dimethoxypyrimidine | HCID 5152323 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzaldehyde, 2-[(4,6-dimethoxy-2-pyrimidinyl)oxy]- | HCID 820623 | 99.9% |
反応手順
A 500-ml four-necked flask was charged with a mixture of 105 g (0.6 mole) of 2-chloro-4,6-dimethoxypyrimidine, 79.4 g (0.65 mole) of salicylic aldehyde, 48.3 g (0.35 mole) of potassium carbonate and 450 ml of dimethylsulfoxide. The mixture was gradually heated, and stirred at 120° C. for 3 hours. After the reaction mixture was cooled, it was poured into 2 l of water. Through the procedures of benzene extraction, washing with water, drying over anhydrous sodium sulfate and concentration, 156 g of the target product were obtained as a crude oil. It was purified further by silica gel chromatography to obtain 117.1 g of white crystals (yield: 75.0%). Melting point: 76.0° about 76.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05053070 |
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| 出典データセット | uspto-grants-1991_10 |
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| ORD ID | ord-e1c7c33a9db2439b820966d43db03769 |
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| 出典メモ | uspto-grants-1991_10 |
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