2-Ethylhexanol → 1,2,4-Benzenetricarboxylic acid, 1(or 2)-(2-ethylhexyl) ester

HRID 620897

反応式

HRID 620897 の反応式
[CH:1]1[C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]2[C:10]([O:12][C:13](=[O:14])[C:3]=2[CH:2]=1)=[O:11].[CH2:15]([CH:17]([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:18][OH:19])[CH3:16].C(O)(=O)C1C(=CC(=CC=1)C(O)=O)C(O)=O>C(CCCO)CCCCO.O[Ti]=O.O>[CH2:15]([CH:17]([CH2:20][CH2:21][CH2:22][CH3:23])[CH2:18][O:19][C:13](=[O:14])[C:3]1[C:4](=[CH:5][C:6](=[CH:1][CH:2]=1)[C:7]([OH:9])=[O:8])[C:10]([OH:12])=[O:11])[CH3:16]

参加物

6

反応物 3

HCID 77202-Ethylhexanol2 回HCID 10708Trimellitic acidHCID 11089Trimellitic anhydride

生成物 1

HCID 1113541,2,4-Benzenetricarboxylic acid, 1(or 2)-(2-ethylhexyl) ester

試薬・触媒・溶媒 2

HCID 21881282Hydroxy(oxo)titanium;octane-1,8-diol触媒HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

193 g (1 mol) of trimellitic acid anhydride and 234 g (1.8 mol) of 2-ethylhexanol plus 0.2 g of octylene glycol titanate were placed in a one-liter round flask. The mixture was heated to 150° C. with stirring and the introduction of nitrogen gas, and the splitting off of water begins. Within 4 hours the temperature is raised to 220° C., the distillate is separated by means of a Vigreux column, the top temperature amounts to 100° to 105° C. The bath temperature is maintained until the top temperature falls below 80° C. The product has an acid number of 150±10 mg KOH/g. 1.7 mol of 2-ethylhexanol per mol of trimellitic acid is contained in the product.

後処理

  1. temperatureWithin 4 hours the temperature is raised to 220° C.
  2. customthe distillate is separated by means of a Vigreux column
  3. customamounts to 100° to 105° C
  4. temperatureThe bath temperature is maintained until the top temperature
  5. customfalls below 80° C

出典と根拠

ORDレコード
ord-b36c82879ac64cc7a1400939de21beac
出典データセット
uspto-grants-1989_04
特許番号
US04822829

関連ノート

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