Acetone → Trimellitic acid

HRID 874797

반응식

HRID 874797 반응식
[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]

참가 물질

5

반응물 4

HCID 180Acetone2회HCID 962WaterHCID 1049PyridineHCID 70998Trimellitic anhydride chloride

생성물 1

HCID 10708Trimellitic acid수율 73%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-63fd847d33a34214b6707bf2814288cf
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08980969B2

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