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

HRID 704137

反応式

HRID 704137 の反応式
[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

参加物

6

反応物 3

HCID 517045Sodium AcetateHCID 118161521,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-HCID 178418287HCID 178418287、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7ab9d0024105477a8aa63b1591117185
出典データセット
uspto-grants-1991_01
特許番号
US04985582

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