Sodium Acetate → 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane

HRID 704137

반응식

HRID 704137 반응식
[CH3:1][C:2]1([CH3:12])[O:7][CH2:6][C:5]([CH2:10][CH3:11])([CH2:8][OH:9])[CH2:4][O:3]1.[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.C([O-])(=O)C.[Na+]>ClCCl.CCOCC>[CH3:1][C:2]1([CH3:12])[O:3][CH2:4][C:5]([CH2:10][CH3:11])([CH:8]=[O:9])[CH2:6][O:7]1

참가 물질

6

반응물 3

HCID 517045Sodium AcetateHCID 118161521,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 120128162,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane수율 92%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

2,2-Dimethyl-5-ethyl-5-hydroxymethyl-1,3-dioxane (33 g.) was added to a stirred suspension of pyridinium chlorochromate (122.6 g) and anhydrous sodium acetate (7.8 g.) in dry dichloromethane (200 ml.), at 0°, under a current of nitrogen. The mixture was stirred at room temperature for six hours. The mixture was diluted with dry ether (500 ml) and the organic solution was decanted off. The oily residue was treated with ether and the combined extracts were evaporated in vacuo. The residue was purified by chromatography on silica, eluting with ether: hexane 1:3. 2,2-Dimethyl-5-ethyl-5-formyl-1,3-dioxane (30 g.) was obtained as a colourless oil.

후처리

  1. customthe organic solution was decanted off
  2. additionThe oily residue was treated with ether
  3. customthe combined extracts were evaporated in vacuo
  4. customThe residue was purified by chromatography on silica
  5. washeluting with ether: hexane 1:3

출처 및 근거

ORD 기록
ord-7ab9d0024105477a8aa63b1591117185
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04985582

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