Methyl Acrylate → 3-Butene-1,2,3-tricarboxylic acid

HRID 26657

反応式

HRID 26657 の反応式
[C:1]([O:5]C)(=[O:4])[CH:2]=[CH2:3].[C:7]([O:16]CC)(=[O:15])/[CH:8]=[CH:9]/[C:10]([O:12]CC)=[O:11]>>[CH2:8]([C:7]([OH:16])=[O:15])[CH:9]([C:10]([OH:12])=[O:11])[C:2]([C:1]([OH:5])=[O:4])=[CH2:3]

参加物

3

実験手順

A mixture of 4.3 parts by weight of methyl acrylate, 7.7 parts by weight of diethyl fumarate and 0.5 parts by weight of diphenyl(4-oxy-butyl)phosphine is boiled and refluxed for 10 hours in a nitrogen stream. Distillation of the reaction product mixture gave a 3-butene-1,2,3-tricarboxylic acid (1,2-diethyl, 3-methyl) ester. The ester of the tricarboxylic acid is converted to a high molecular weight carboxylic acid-producing composition by reacting same with a chlorinated polyisobutene having a molecular weight of about 1000 and a chlorine content of about 4.5% at a temperature ranging from about 80°-120° C. A mixture of approximately 2000 parts by weight of mineral oil, 3.0 equivalents of a polyoxyethylene triamine having an average molecular weight of about 1000 and approximately 3.0 equivalents of the above-mentioned high molecular weight tricarboxylic acid-producing composition is heated to temperatures of 150°-200° C. over a period of 15 to 20 hours. The resulting product is filtered to give a homogeneous mineral oil solution of the acylated polyamine.

後処理

  1. temperaturerefluxed for 10 hours in a nitrogen stream
  2. distillationDistillation of the reaction product mixture

出典と根拠

ORDレコード
ord-a8a393e392804dc2ad5bfa52ca98aebb
出典データセット
uspto-grants-1979_04
特許番号
US04151173

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