3-(Cyclohexyloxy)propan-1-ol → HCID 22279671、化合物

HRID 1063469ノート

反応式

HRID 1063469 の反応式
[CH:1]1([O:7][CH2:8][CH2:9][CH2:10][OH:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl.CCOCC>[CH:1]1([O:7][CH2:8][CH2:9][CH:10]=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 100348783-(Cyclohexyloxy)propan-1-olHCID 178418287HCID 178418287、化合物

生成物 1

HCID 22279671HCID 22279671、化合物収率 75.5%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

The obtained 3-cyclohexyloxypropan-1-ol (11.5 g, 72.9 mmol) was dissolved in dichloromethane (240 ml), and then molecular sieve 4 Å (58 g) and pyridinium chlorochromate (23.8 g, 0.11 mol) were added thereto in the ice bath followed by stirring under a nitrogen atmosphere for 1 hour and 40 minutes. The reaction solution was diluted with ether, and then the solution was filtered through Celite. The Celite was washed with diethyl ether, and this filtrate was added to the previous filtrate. The total filtrate was evaporated in vacuo, and the residue was purified roughly by chromatography on a silica gel column (elution solvent; n-hexane:ethyl acetate=20:1-10:1) to give a crude 3-cyclohexyloxypropionaldehyde (8.6 g).

後処理

  1. filtrationthe solution was filtered through Celite
  2. washThe Celite was washed with diethyl ether
  3. additionthis filtrate was added to the previous filtrate
  4. customThe total filtrate was evaporated in vacuo
  5. customthe residue was purified roughly by chromatography on a silica gel column (elution solvent; n-hexane:ethyl acetate=20:1-10:1)

出典と根拠

ORDレコード
ord-8dae63e5e5a747458a25a77ee2fd048f
出典データセット
uspto-grants-2005_11
特許番号
US06964976B2

反応ノート

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