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4-Chlorobenzoic Acid → 4,4'-Oxydiphthalic anhydride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chlorobenzoic Acid | HCID 6318 | — |
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chlorophthalic anhydride | HCID 67044 | — |
| 触媒 | Tetraphenylphosphonium Bromide | HCID 2724163 | — |
| 生成物 | 4,4'-Oxydiphthalic anhydride | HCID 74574 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05153335 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-1f4db03b584f49bba0584bfca4a5bd52 |
| 出典メモ | uspto-grants-1992_10 |