関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyruvic Acid | HCID 1060 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2',5-dichloro-3-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide | HCID 21325684 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2',5-dichloro-3-(3-pyruvamidomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone | HCID 21325744 | 64.8% |
反応手順
A solution of pyruvic acid (0.33 g) and thionyl chloride (0.27 g) in chloroform (2 ml) is refluxed for 1 hour. After cooling, the solution is mixed with 2',5-dichloro-3-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide (1.31 g), benzene (6 ml) and dimethylformamide (11 ml) at 0° C. The resultant mixture is stirred at room temperature for 3 hours and allowed to stand overnight. The reaction mixture is neutralized with aqueous sodium bicarbonate and shaken with ethyl acetate. The organic layer is washed with water, dried and evaporated to remove the solvent. The residue is recrystallized from ethyl acetate to give 2',5-dichloro-3-(3-pyruvamidomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone (0.7 g) as crystals melting at 178° to 180° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04147700 |
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| 出典データセット | uspto-grants-1979_04 |
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| ORD ID | ord-9ffa1233d3a54301a7b399e8045faf43 |
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| 出典メモ | uspto-grants-1979_04 |
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