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

HRID 850987
ノート
印刷プレビュー

反応式

HRID 850987 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
溶媒
2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a3bb02f5210c4453bea26f0161225774
出典データセット
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04382143

反応ノート

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