Ethylene Glycol → Tertiary butoxymethyl diethylene glycol

HRID 127665

反応式

HRID 127665 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 20285608Tertiary butoxymethyl diethylene glycol収率 71%

試薬・触媒・溶媒 2

HCID 8000Boron trifluoride etherate触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-203857138ae24d558113da98a74e02ca
出典データセット
uspto-grants-1981_03
特許番号
US04256859

関連ノート

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