Ethylene Glycol → Tertiary butoxymethyl diethylene glycol

HRID 127665

반응식

HRID 127665 반응식
[CH2:1]([OH:4])[CH2:2][OH:3].[CH3:5][C:6]([O:9][CH2:10][CH:11]1[O:13][CH2:12]1)([CH3:8])[CH3:7].[OH-].[Na+]>B(F)(F)F.CCOCC.ClCCl>[C:6]([O:9][CH2:10][CH:11]([OH:13])[CH2:12][O:3][CH2:2][CH2:1][OH:4])([CH3:5])([CH3:7])[CH3:8]

참가 물질

6

반응물 3

HCID 174Ethylene GlycolHCID 14798Sodium HydroxideHCID 243142-((1,1-Dimethylethoxy)methyl)oxirane

생성물 1

HCID 20285608Tertiary butoxymethyl diethylene glycol수율 71%

시약·촉매·용매 2

HCID 8000Boron trifluoride etherate촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of ethylene glycol (248 g, 4 moles) and boron trifluoride etherate catalyst (1 ml) in dichloromethane (20 ml) preheated to 45° C. was added t-BGE (130 g, 1 mole) dropwise at such a rate so as to maintain a gentle reflux. After completion of addition, stirring was continued for about 15 hours. The solution was then adjusted to pH 7.5 by addition of sodium hydroxide and the product removed by distillation. Tertiary butoxymethyl diethylene glycol was obtained in 71 percent yield having a boiling point of 105° C.-115° C./1 mm.

후처리

  1. custompreheated to 45° C.
  2. temperatureto maintain a gentle reflux
  3. additionAfter completion of addition
  4. customthe product removed by distillation

출처 및 근거

ORD 기록
ord-203857138ae24d558113da98a74e02ca
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256859

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