Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Phenol | HCID 996 | — |
| Edukt | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | — |
| Katalysator | Titanium tetraphenoxide phenol | HCID 86752029 | — |
| Produkt | Benzoic acid, 3,5-dimethyl-, methyl ester | HCID 32786 | — |
| Produkt | Phenyl 3,5-dimethylbenzoate | HCID 19704462 | — |
Reaktionsschritte
Into this autoclave were charged methyl 3,5-dimethylbenzoate 90 g (550 mmole), phenol 207 g (2200 mmole) and titanium tetraphenoxide/phenol adduct 2.8 g (5.5 mmole) in a state such that the phenol was melting. The autoclave was sealed and then cooled with ice. After sufficient cooling, the inner gas was evacuated with a vacuum pump. Then, the contents were heated and reacted for three hours at 230° C. Furthermore, during the reaction, the liquid held in the reservoir was continuously removed with a pump at a rate of 10 g per hour. After cooling, the reaction mixture in the autoclave was separated by distillation to obtain phenyl 3,5-dimethylbenzoate (product) in an amount of 85 g (68% yield in terms of methyl 3,5-dimethylbenzoate). The boiling point was 155° C./2 mmHg, and the melting point was 32° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05714627 |
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| Quelldatensatz | uspto-grants-1998_02 |
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| ORD ID | ord-e6cbd8c2ee7a4e58a36f8c4288f0b247 |
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| Quellennotiz | uspto-grants-1998_02 |
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