関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzaldehyde | HCID 240 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | 3-(Dimethylamino)-1-phenyl-1-propanone | HCID 77042 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Diphenyl-2-methyl-1,3-propandione | HCID 344637 | — |
反応手順
A solution of 21.2 g (0.2 mol) of benzaldehyde and 100 ml of absolute dimethylformamide is added dropwise in the course of 1/2 hour to a mixture of 9.8 g (0.2 mol) of NaCN and 100 ml of absolute dimethylformamide in a manner analogous to Example 3. Stirring is continued for 21/2 hours at 35° C. A solution of 26.6 g (0.15 mol) of dimethyl-β-benzoyl-ethylamine and 100 ml of absolute dimethylformamide is then slowly added dropwise in the course of 2 hours. Stirring is continued for 2 hours at the same temperature and water is then added to the reaction mixture in three times its quantity. The reaction product precipitates immediately. After cooling in an ice bath, the precipitated product is suction filtered and thoroughly washed with water. 34.3 g of crude product are isolated. 21.6 g (60.5% of the theory) of dibenzoyl ethane are isolated by recrystallisation from ethanol; m.p. 143° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04014889 |
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| 出典データセット | uspto-grants-1977_03 |
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| ORD ID | ord-1edd11de3330483aa6ca975150942e01 |
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| 出典メモ | uspto-grants-1977_03 |
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