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

HRID 1739773

반응식

HRID 1739773 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d18f2ce5649c497b8892fb78a99ce117
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05968947

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