Sodium sulfate decahydrate → tert-Butyl (3R)-3-(2-hydroxyethyl)piperidine-1-carboxylate

HRID 1761179ノート

反応式

HRID 1761179 の反応式
C([O:3][C:4](=O)[CH2:5][C@H:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[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][C@H:6]1[CH2:11][CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7]1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 29919087(R)-1-Boc-3-piperidine acetate ethyl ester

生成物 1

HCID 40425180tert-Butyl (3R)-3-(2-hydroxyethyl)piperidine-1-carboxylate収率 97.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 143 mg of t-butyl(3R)-3-(2-ethoxy-2-oxoethyl)tetrahydropyridine-1(2H)-carboxylate in 5 ml of tetrahydrofuran, 30 mg of litiumaluminum 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 12 hours and filtered with Celite. Distilling the solvent off under reduced pressure, 118 mg of the title compound was obtained.

後処理

  1. temperatureunder cooling with ice
  2. additionwas added
  3. stirringstirred for 12 hours
  4. filtrationfiltered with Celite
  5. distillationDistilling the solvent off under reduced pressure

出典と根拠

ORDレコード
ord-1dd0d357d23e4e5585affb32963645e5
出典データセット
uspto-grants-2005_01
特許番号
US06846835B2

反応ノート

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