Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Terephthalic Acid | HCID 7489 | — |
| Reactant | Fuming sulfuric acid | HCID 24681 | — |
| Reactant | CID 19593658 | HCID 19593658 | — |
| Product | HCID 68486048 | HCID 68486048 | — |
Reaction Steps
Oleum (25% SO3, 95 ml) is charged into a reactor (350 ml). Under stirring terephthalic acid (19.0 g; 0.11 mol) is added to the reactor and the mixture is heated to 60° C. After stirring for additional 30 min terephthalic acid (31.0 g; 0.19 mol) is added and the mixture is heated to 100° C. for 1 hour. The mixture is cooled to 25-30° C., trioxane (12.0 g; 0.13 mol) is added in portions and the reaction mixture is heated slowly to 130-135° C. and agitated at this temperature for 1½ hours and for 4 hours at 155° C. The reaction mixture is cooled to 40° C. and added to a reactor containing butanol (150 ml) and heptanes (150 ml) witch has been heated to 95-100° C. The formed precipitates were diluted with butanol (85 ml) and stirring overnight. The precipitate is filtered off and dried.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07687645B2 |
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| Source dataset | uspto-grants-2010_03 |
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| ORD ID | ord-18997bf42da54f6181c2952a9a40e6eb |
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| Source note | uspto-grants-2010_03 |
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