関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 2,5-Bis(2,2,2-trifluoroethoxy)-N-(2-pyridylmethyl)benzamide | HCID 93669 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Flecainide Acetate | HCID 41022 | 71% |
反応手順
A mixture of 0.33 mole (134.7 g.) 2,5-bis(2,2,2-trifluoroethoxy)-N-(2-pyridylmethyl)benzamide, 1.347 liter of glacial acetic acid and 13.5 g. of 5 percent platinum on carbon is reduced in a Parr apparatus at a pressure of about 10 pounds of hydrogen at room temperature. The reaction is complete in 6-7 hours. The reaction mixture is filtered and the catalyst is washed with isopropyl alcohol. The solution and washings are evaporated to provide a residue. Hexane is added to the residue and the resulting white solid is collected and recrystallized from a mixture of acetone and hexane. A 71 percent yield of 2,5-bis(2,2,2-trifluoroethoxy)-N-(2-piperidylmethyl)benzamide acetate, m.p. 150° to 152° C., is obtained. By concentrating the residual liquid an additional 18 percent of product is obtained as a second crop with a melting point of 148°-150° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04617396 |
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| 出典データセット | uspto-grants-1986_10 |
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| ORD ID | ord-7c24eb96b9e84c3bb1db397eb5c43c46 |
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| 出典メモ | uspto-grants-1986_10 |
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