関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-(4-Chloro-3-(trifluoromethyl)phenyl)piperidin-4-ol | HCID 89107 | — |
| 反応物 | (Dihydro-3,3-diphenyl-3H-furan-2-ylidene)dimethylammonium bromide | HCID 2723589 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Methyl Isobutyl Ketone | HCID 7909 | — |
| 生成物 | Fluperamide hydrochloride | HCID 214899 | — |
反応手順
A mixture of 12.1 parts of dimethyl (tetrahydro-3,3-diphenyl-2-furylidene) ammonium bromide, 8.4 parts of 4-(4-chloro-3-trifluoromethylphenyl)-4-piperidinol, 8 parts of sodium carbonate, 0.4 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 3 hours with water separator. The reaction mixture is cooled and water is added. The organic layer is separated, washed with diluted sodium hydroxide solution, dried and concentrated to a volume of about 200 parts. The concentrate is acidified with an excess of 2-propanol previously saturated with gaseous hydrogen chloride. Upon stirring, the salt is crystallized. It is filtered off and dried, yielding 4-(4-chloro-3-trifluoromethylphenyl)-4-hydroxy-N,N-dimethyl-α,α-diphenylpiperidine-1-butyramide hydrochloride; m.p. 215.3° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05811078 |
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| 出典データセット | uspto-grants-1998_09 |
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| ORD ID | ord-126a5484f7104d208acb7d7370da4a4f |
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| 出典メモ | uspto-grants-1998_09 |
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