Ethylene Glycol → Methyl 4,4-ethylenedioxy-3-methyl-butanoate

HRID 2051726ノート

反応式

HRID 2051726 の反応式
[CH3:1][CH:2]([CH:8]=[O:9])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[CH2:10](O)[CH2:11][OH:12].C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>CCOCC>[CH2:10]1[CH2:11][O:12][CH:8]([CH:2]([CH3:1])[CH2:3][C:4]([O:6][CH3:7])=[O:5])[O:9]1

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 11804788Methyl 3-methyl-4-oxobutanoate

生成物 1

HCID 20305753Methyl 4,4-ethylenedioxy-3-methyl-butanoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of methyl 3-methyl-4-oxo-butanoate (86.3 g), ethylene glycol (61.75 g, 0.996 m), p-toluenesulfonic acid (1 g) and benzene (700 ml) is refluxed under nitrogen for 16 hr. The resulting mixture is allowed to cool to room temperature and treated with ether (300 ml). The organic phase is washed with 5% sodium bicarbonate solution (100 ml), dried (Na2SO4) and evaporated in vacuo to give methyl 4,4-ethylenedioxy-3-methyl-butanoate as a crude product (63.2 g). This material is used directly in the next step.

後処理

  1. temperatureis refluxed under nitrogen for 16 hr
  2. washThe organic phase is washed with 5% sodium bicarbonate solution (100 ml)
  3. dry with materialdried (Na2SO4)
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-c30988f0051a47189587616052ccb2d1
出典データセット
uspto-grants-1980_01
特許番号
US04182717

反応ノート

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