Sodium sulfate decahydrate → 1-(tert-Butoxycarbonyl)-4-(2-hydroxyethyl)piperidine

HRID 458754노트

반응식

HRID 458754 반응식
C([O:3][C:4](=O)[CH2:5][CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[OH:3][CH2:4][CH2:5][CH:6]1[CH2:7][CH2:8][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:10][CH2:11]1

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 9993342Ethyl 1-((1,1-dimethylethoxy)carbonyl)-4-piperidineacetateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 8541401-(tert-Butoxycarbonyl)-4-(2-hydroxyethyl)piperidine수율 93.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 263 mg of t-butyl 4-(2-ethoxy-2-oxoethyl)-tetrahydropyridine-1(2H)-carboxylate in 15 ml of tetrahydrofuran, 100 mg of lithiumaluminum hydride was added under cooling with ice, followed by 20 minutes' stirring at the same temperature. To the reaction liquid sodium sulfate decahydrate was added, stirred for 30 minutes and filtered with Celite. Distilling the solvent off under reduced pressure, 207 mg of the title compound was obtained.

후처리

  1. temperatureunder cooling with ice
  2. additionwas added
  3. stirringstirred for 30 minutes
  4. filtrationfiltered with Celite
  5. distillationDistilling the solvent off under reduced pressure

출처 및 근거

ORD 기록
ord-95321922b76748fd9e7d076eceb7b817
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192969B2

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