関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Piperidine-2-methylamine | HCID 90865 | — |
| 反応物 | 2,2,2-Trifluoroethyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate | HCID 11281014 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Flecainide | HCID 3356 | — |
反応手順
Dissolve in 48 ml of toluene 12.0 g (0.03 mol) of trifluoroethanol 2,5-bis-trifluoroethoxybenzoate. Add 3.94 g (0.0345 mol) of 2-aminomethylpiperidine and heat the solution to a temperature of 80°±5° C. for 8 hours. Cool to 50° C. and add 36 ml of water. Carry out the separation at a temperature of 45°±5° C. Concentrate the organic phase under vacuum at a temperature of 35°±5° C. so as to eliminate as much toluene as possible. A semi-solid residue is obtained which is dissolved in 20 ml of methanol and concentrated again to a residue under vacuum. Methanol (40 ml) is then added and heated with refluxing until a yellow solution is obtained. Then cool until the crude base crystallizes, the precipitation is completed by adding 40 ml of water.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06599922B2 |
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| 出典データセット | uspto-grants-2003_07 |
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| ORD ID | ord-fd062efa44324b67b5831a945dd1e406 |
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| 出典メモ | uspto-grants-2003_07 |
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