4-Chlorobenzoic Acid → 4,4'-Oxydiphthalic anhydride

HRID 465739

반응식

HRID 465739 반응식
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[O:10])[O:8][C:6](=[O:7])[C:5]2=[CH:11][CH:12]=1.[C:13](=[O:16])([O-:15])[O-].[K+].[K+].Cl[C:20]1[CH:28]=[CH:27][C:23]([C:24](O)=[O:25])=[CH:22][CH:21]=1.[N+](C1C=CC=CC=1)([O-])=[O:30]>[Br-].C1([P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH:12]1[C:2]([O:30][C:28]2[CH:20]=[CH:21][C:22]3[C:13]([O:15][C:24](=[O:25])[C:23]=3[CH:27]=2)=[O:16])=[CH:3][C:4]2[C:9]([O:8][C:6](=[O:7])[C:5]=2[CH:11]=1)=[O:10]

참가 물질

6

반응물 4

HCID 63184-Chlorobenzoic AcidHCID 7416Nitrobenzene2회HCID 11430Potassium Carbonate2회HCID 670444-Chlorophthalic anhydride

생성물 1

HCID 745744,4'-Oxydiphthalic anhydride

시약·촉매·용매 1

HCID 2724163Tetraphenylphosphonium Bromide촉매

실험 절차

4-Chlorophthalic anhydride (30 g, 160 mmol), and nitrobenzene (Aldrich, 30 g, containing 500 ppm water) were heated to reflux. Dry potassium carbonate (1.32 g, 9.6 mmol) was added and the mixture heated for 30 minutes. Tetraphenyl phosphonium bromide (0.36 g, 0.9 mmol) and 4-chlorobenzoic acid (0.06 g, 0.4 mmol) were added followed by addition of potassium carbonate (11.4 g, 82.2 mmol). The reaction was heated for about 9 hours and then was diluted with nitrobenzene (30 g) and filtered. The 4,4'-oxydiphthalic anhydride was allowed to crystallize, was washed with solvent, and dried in an air circulating oven at 120° C. to give crude 4,4'-oxydiphthalic anhydride, 10.0 g.

후처리

  1. temperaturethe mixture heated for 30 minutes
  2. temperatureThe reaction was heated for about 9 hours
  3. filtrationfiltered
  4. customto crystallize
  5. washwas washed with solvent
  6. customdried in an air
  7. customat 120° C.

출처 및 근거

ORD 기록
ord-1f4db03b584f49bba0584bfca4a5bd52
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05153335

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