3-(Cyclohexyloxy)propan-1-ol → HCID 22279671, 화합물

HRID 1063469노트

반응식

HRID 1063469 반응식
[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

참가 물질

5

반응물 2

HCID 100348783-(Cyclohexyloxy)propan-1-olHCID 178418287HCID 178418287, 화합물

생성물 1

HCID 22279671HCID 22279671, 화합물수율 75.5%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-8dae63e5e5a747458a25a77ee2fd048f
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06964976B2

반응 노트

불러오는 중…