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

HRID 620315

반응식

HRID 620315 반응식
[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]

참가 물질

6

반응물 3

HCID 77202-Ethylhexanol2회HCID 10708Trimellitic acidHCID 11089Trimellitic anhydride

생성물 1

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

시약·촉매·용매 2

HCID 21881282Hydroxy(oxo)titanium;octane-1,8-diol촉매HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

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 amount to 100° to 150° 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.

후처리

  1. temperatureWithin 4 hours the temperature is raised to 220° C.
  2. customthe distillate is separated by means of a Vigreux column
  3. customto 100° to 150° C
  4. temperatureThe bath temperature is maintained until the top temperature
  5. customfalls below 80° C

출처 및 근거

ORD 기록
ord-c0c7ee24ad8b48d7859e6252cfb168c2
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04820745

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