関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Calciumoxide | HCID 6850728 | — |
| 反応物 | HCID 13742658 | HCID 13742658 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 3,3'-Diaminobenzophenone | HCID 69145 | — |
反応手順
In an autoclave, there are charged 46 g (0.15 moles) of 3,3'-dinitro-4-chloro benzophenone, 11.2 g (0.2 moles) of calcium oxide, 1 g of 5% palladium/alumina catalyst (available from Nihon-Engelhardt Co.) and 250 ml of 1,2-dichloro ethane. With the mixture being stirred at a temperature of 30°-35° C., the reaction proceeds by the introduction of hydrogen for seven hours under a constant pressure of 10 Kg/cm2.G. After completion of the reaction, the reaction mixture is heated up to 70° C. for hot-filtering so as to remove the catalyst and the inorganic salt. On cooling, there is obtained 3,3'-diamino benzophenone as yellow needle-like crystals. The crystals are filtered, washed with 20 ml of 1,2-dichloro ethane and dried. Yield 24.8 g (78%). M.P. 149°-150° C. Recrystallization from ethanol gives yellow needle-like pure crystals of the benzophenone. M.P. 150°-151° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04556738 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-393fdd5624b94bcea943633e3d048f7e |
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| 出典メモ | uspto-grants-1985_12 |
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