Potassium Iodide → 1,1'-Oxybis(2,2-diethoxyethane)

HRID 1596329ノート

反応式

HRID 1596329 の反応式
[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][OH:6])[CH3:2].[H-].[Na+].[CH2:12]([O:14][CH:15]([O:18][CH2:19][CH3:20])[CH2:16]Br)[CH3:13].[I-].[K+]>O1CCCC1.O>[CH2:1]([O:3][CH:4]([O:7][CH2:8][CH3:9])[CH2:5][O:6][CH2:16][CH:15]([O:18][CH2:19][CH3:20])[O:14][CH2:12][CH3:13])[CH3:2]

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 121292,2-DiethoxyethanolHCID 24758Sodium hydrideHCID 74852Ethane, 2-bromo-1,1-diethoxy-

生成物 1

HCID 926201,1'-Oxybis(2,2-diethoxyethane)

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Hydroxyacetaldehyde diethylacetal (3.75 g) was added to sodium hydride (0.8 g, 80% in mineral oil) in tetrahydrofuran (100 ml) under an atmosphere of nitrogen. The mixture was stirred and bromoacetaldehyde diethyl acetal (5.0 g) and potassium iodide (0.1 g) were added. The mixture was heated to reflux for 16 hours, water added and evaporated under reduced pressure. The residue was dissolved in diethyl ether, the organic phase washed with water, dried (MgSO4) and evaporated under reduced pressure to give bis(2,2-diethoxyethyl)ether, 3.43 g, as a yellow oil.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 16 hours
  3. customevaporated under reduced pressure
  4. dissolutionThe residue was dissolved in diethyl ether
  5. washthe organic phase washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-762dd13dd60b46679156dd68420a4155
出典データセット
uspto-grants-2001_09
特許番号
US06291474B1

反応ノート

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