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

HRID 465739

反応式

HRID 465739 の反応式
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]

参加物

6

反応物 4

HCID 63184-Chlorobenzoic AcidHCID 7416Nitrobenzene2 回HCID 11430Potassium Carbonate2 回HCID 670444-Chlorophthalic anhydride

生成物 1

HCID 745744,4'-Oxydiphthalic anhydride

試薬・触媒・溶媒 1

HCID 2724163Tetraphenylphosphonium Bromide触媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-1f4db03b584f49bba0584bfca4a5bd52
出典データセット
uspto-grants-1992_10
特許番号
US05153335

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