Water → HCID 22135707、化合物

HRID 344288

反応式

HRID 344288 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](OCC)=[O:15])[C:10](=[O:19])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[BH4-].[Na+].O>C(O)C>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][OH:15])[CH:10]([OH:19])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 419705Ethyl 3-oxo-1-(phenylmethyl)-4-piperidinecarboxylateHCID 4311764Sodium borohydride

生成物 1

HCID 22135707HCID 22135707、化合物収率 59.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of ethyl 1-benzyl-3-oxo-4-piperidinecarboxylate (21 g) in ethanol (20 ml) was added sodium borohydride (9.1 g) under ice-cooling, and the resulting mixture was stirred at room temperature for 9 hr. Water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with brine and dried. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography to give 10.55 g of 1-benzyl-3-hydroxy-4-hydroxymethylpiperidine.

後処理

  1. temperaturecooling
  2. extractionthe mixture was extracted with chloroform
  3. washThe organic layer was washed with brine
  4. customdried
  5. customThe solvent was evaporated under reduced pressure
  6. customthe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-1a7410ce394c4b899bbfaa28899ba484
出典データセット
uspto-grants-1999_01
特許番号
US05864039

関連ノート

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