Acetone → Trimellitic acid

HRID 874797

Reaktionsgleichung

Reaktionsgleichung von HRID 874797
[CH:1]1[C:6]([C:7](Cl)=[O:8])=[CH:5][C:4]2[C:10]([O:12][C:13](=[O:14])[C:3]=2[CH:2]=1)=[O:11].N1C=CC=CC=1.[OH2:21].CC(C)=[O:24]>>[C:13]([OH:12])(=[O:14])[C:3]1[C:4](=[CH:5][C:6](=[CH:1][CH:2]=1)[C:7]([OH:24])=[O:8])[C:10]([OH:11])=[O:21]

Komponenten

5

Edukt 4

HCID 180Acetone2×HCID 962WaterHCID 1049PyridineHCID 70998Trimellitic anhydride chloride

Produkt 1

HCID 10708Trimellitic acidAusbeute 73 %

Versuchsvorschrift

Trimellitic acid anhydride chloride (32.40 g, 0.154 mol) was dissolved 100 mL acetone in a 3-neck flask under nitrogen. The flask was cooled in an ice bath. The solution was stirred continuously while a solution of AFM-1 (35.25 g, 0.0773 mol), and pyridine (12.32 g, 0.154 mol) in 50 ml of acetone was added slowly to the cold solution using a dropping funnel. After addition was completed, the flask contents were continuously stirred at room temperature for 4 hours. Water (2.77 g, 0.154 mol) was added and stirring at room temperature was continued overnight. Then the solid formed was removed by vacuum filtration and washed with acetone. The filtrate was concentrated and dried to a white solid with 73% yield. The structure confirmed by NMR.

Aufarbeitung

  1. temperatureThe flask was cooled in an ice bath
  2. additionwas added slowly to the cold solution
  3. additionAfter addition
  4. stirringstirring at room temperature
  5. waitwas continued overnight
  6. customThen the solid formed
  7. customwas removed by vacuum filtration
  8. washwashed with acetone
  9. concentrationThe filtrate was concentrated
  10. customdried to a white solid with 73% yield

Quellen und Nachweise

ORD-Eintrag
ord-63fd847d33a34214b6707bf2814288cf
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08980969B2

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