Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | O-Xylene | HCID 7237 | — |
| Reactant | Bicyclo(2.2.1)hept-5-ene-2-methanol | HCID 78946 | — |
| Reactant | 3-(3,4-Difluorophenyl)prop-2-enoic acid | HCID 145486 | — |
| Catalyst | HCID 86657292 | HCID 86657292 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86657294 | HCID 86657294 | 63% |
Reaction Steps
5 g (27.2 mmol) of 3,4-di-fluoro-cinnamic acid, 3.38 g (1 eq.) of 5-norbornene-2-methanol, and 0.13 g (0.02 eq.) of zirconium(IV) acetate hydroxide were added to 50 ml of xylene and stirred. The mixture was heated to 145° C. under N2 atmosphere and azeotropically refluxed for 24 hours. After the reaction, the mixture cooled down to room temperature and was added with 100 volume % of ethyl acetate. The resulting product was extracted by 1M HCl and washed again with water. The organic layer was dried with Na2SO4 and the solvent was evaporated out to give a highly viscous material. (Yield: 63%, Purity (GC): 80%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08231946B2 |
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| Source dataset | uspto-grants-2012_07 |
|---|
| ORD ID | ord-935c33ad87454981a088fceb99e11a01 |
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| Source note | uspto-grants-2012_07 |
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