참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3-amino-N-ethylpiperidine | HCID 98094 | — |
| 반응물 | 2-(8-Trifluoromethyl-4-quinolylamino)benzoic acid hydrochloride dihydrate | HCID 70546379 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | Thionyl Chloride | HCID 24386 | — |
| 생성물 | N-(1-Ethyl-3-piperidyl)-2-(8-trifluoromethyl-4-quinolylamino)benzamide | HCID 20520121 | 63% |
반응 단계
11.5 Grams (0.0285 Mole) of 2-(8-trifluoromethyl-4-quinolylamino)benzoic acid hydrochloride dihydrate were refluxed in 80 milliliters of thionyl chloride for half an hour. A yellow solid precipitated. The thionyl chloride was evaporated off. The resulting acid chloride hydrochloride was added in portions with stirring to a cooled mixture of 3.84 grams (0.03 moles) of 3-amino-1-ethylpiperidine in 100 milliliters of chloroform and 31.8 grams (0.3 mole) of sodium carbonate in 100 milliliters of water. The mixture was stirred for one hour and allowed to stand overnight. The chloroform layer was separated and dried and the chloroform evaporated to give a nearly colourless solid. Trituration with ether gave a colourless solid which was recrystallized from methanol to give 7.9 grams (63% yield) of title compound, melting point 212° to 213° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04357333 |
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| 출처 데이터셋 | uspto-grants-1982_11 |
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| ORD ID | ord-1430adf7fcdc446a94db511eb348b9a1 |
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| 출처 메모 | uspto-grants-1982_11 |
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