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Piperidine → 1-(4-Hexadecylamino-2-thiophenecarbonyl)piperidine

HRID 850987
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인쇄 미리보기

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HRID 850987 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.CN(C1C=CC=CN=1)C.Cl.[CH2:24]([NH:40][C:41]1[CH:42]=[C:43]([C:46](Cl)=[O:47])[S:44][CH:45]=1)[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39]>CCOCC>[CH2:24]([NH:40][C:41]1[CH:42]=[C:43]([C:46]([N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[O:47])[S:44][CH:45]=1)[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8082PiperidineHCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 205036504-Hexadecylamino-2-thiophenecarbonyl chloride hydrochloride

생성물 1

HCID 205036111-(4-Hexadecylamino-2-thiophenecarbonyl)piperidine

시약·촉매·용매 1

HCID 3283Diethyl Ether
용매
2회

실험 절차

To a chilled solution of 35 ml. of piperidine, 2.5 ml. of triethylamine and 0.6 g. of dimethylaminopyridine in 100 ml. of diethyl ether is added (1/2 hour) a solution of 8.3 g. of 4-hexadecylamino-2-thiophenecarbonyl chloride hydrochloride in 50 ml. of ether. The solution is warmed to room temperature and maintained there for two hours. The solution is heated to reflux for an additional 2 hours at which time the reaction is complete. The solution is cooled, extracted twice with water and dried. The solvent is removed in vacuo and the solid is recrystallized from ether to yield the product as a white solid.

후처리

  1. temperaturemaintained there for two hours
  2. temperatureThe solution is heated
  3. temperatureto reflux for an additional 2 hours at which time the reaction
  4. temperatureThe solution is cooled
  5. extractionextracted twice with water
  6. customdried
  7. customThe solvent is removed in vacuo
  8. customthe solid is recrystallized from ether

출처 및 근거

ORD 기록
ord-a3bb02f5210c4453bea26f0161225774
출처 데이터셋
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04382143

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