関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | (Z)-Benzaldehyde oxime | HCID 12143 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-4'-nitrobenzophenone | HCID 347771 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-Hydroxy-4'-chlorobenzophenone | HCID 123504 | — |
反応手順
250 cc of DMSO and 4.8 g sodium hydride are placed in a 500 cc flask and heated at 70° C. for 1 hour, by which time the solution has become clear. A solution of 24.2 g (0.2 mole) of benzaldoxime in 100 cc of DMSO is then added drop by drop. The solution is maintained at 70° C. for 1 hour, then allowed to cool to 15° C. A solution of 26 g (0.1 mole) of 4'-chloro-4-nitrobenzophenone in 150 cc of DMSO is then added. The reaction mixture is stirred for 20 hours at ambient temperature and then poured into acidulated water. The mixture is extracted with ether and then with ether containing 2 N caustic soda. On acidification the product is precipitated. Yield 15 g (65%). Melting point 178° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04235896 |
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| 出典データセット | uspto-grants-1980_11 |
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| ORD ID | ord-37898582841347cfa55f6a3527a44f0a |
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| 出典メモ | uspto-grants-1980_11 |
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