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

HRID 458754ノート

反応式

HRID 458754 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-95321922b76748fd9e7d076eceb7b817
出典データセット
uspto-grants-2007_03
特許番号
US07192969B2

反応ノート

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