Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Terephthalic Acid | HCID 7489 | — |
| Reactant | CID 19593658 | HCID 19593658 | — |
| Solvent | Fuming sulfuric acid | HCID 24681 | — |
| Product | Phthalide | HCID 6885 | — |
Reaction Steps
Terephthalic acid was suspended in 25-30% oleum. Trioxane was added and the mixture was heated to 140-150° C. for 4-8 hours. The reaction mixture was cooled and then quenched by cautious addition of water at less than 80° C. The resulting suspension was cooled to about 40° C. and the solid was filtered off. The filter cake was washed with water followed by propan-2-ol before slurrying the solid in propan-2-ol at reflux for 30 minutes. After cooling to 20-25° C. the product was filtered off, washed with propan-2-ol and dried at 60-70° C. under reduced pressure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07002025B2 |
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| Source dataset | uspto-grants-2006_02 |
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| ORD ID | ord-543a51228027465599b2934133cb5483 |
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| Source note | uspto-grants-2006_02 |
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