2,2-Diethoxyethanol → 1,1'-Oxybis(2,2-diethoxyethane)

HRID 1355371

反応式

HRID 1355371 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]>C1(C)C(C)=CC=CC=1>[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

5

反応物 3

HCID 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 1

HCID 7237O-Xylene溶媒

実験手順

Glycolaldehyde diethyl acetal (45.4 g, 338 mmol) was added dropwise to a stirred solution of sodium hydride (14.3 g, 60% dispersion in mineral oil, 357 mmol) in xylene (100 ml), and the reaction heated under reflux for 1 hour. The reaction mixture was cooled to room temperature and bromoacetaldehyde diethyl acetal (100 g, 507 mmol) was added. The resulting solution was heated under reflux for 20 hours, then cooled to room temperature. The solvent was removed under reduced pressure, and the residual solution was distilled under reduced pressure (80° C. @ 6 mm Hg), to afford the title compound as a colourless oil, 60.8 g.

後処理

  1. temperaturethe reaction heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe resulting solution was heated
  4. temperatureunder reflux for 20 hours
  5. temperaturecooled to room temperature
  6. customThe solvent was removed under reduced pressure
  7. distillationthe residual solution was distilled under reduced pressure (80° C. @ 6 mm Hg)

出典と根拠

ORDレコード
ord-0a65254ebd624fac88975dec0d601453
出典データセット
uspto-grants-2003_07
特許番号
US06586430B1

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