참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Piperidine-2-methylamine | HCID 90865 | — |
| 반응물 | 2,2,2-Trifluoroethyl 2,5-bis(2,2,2-trifluoroethoxy)benzoate | HCID 11281014 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Flecainide | HCID 3356 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06599922B2 |
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| 출처 데이터셋 | uspto-grants-2003_07 |
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| ORD ID | ord-fd062efa44324b67b5831a945dd1e406 |
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| 출처 메모 | uspto-grants-2003_07 |
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