Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | HCID 86722243 | HCID 86722243 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86722244 | HCID 86722244 | 19.2% |
Reaction Steps
To a mixture of 11E (2.6 g, 6.19 mmol) in MeCN (30 mL) was added ZnCl2 (1.27 g, 1.5 eq, 9.3 mmol) at room temperature, followed by AcOH (30 mL) and H3PO4 (30 mL) The reaction mixture was stirred 80° C. overnight. After reaction completed, the mixture was cooled and poured into crushed ice under stirring, neutralized to pH=7˜8, extracted with ethyl acetate, dried and concentrated to give 1.6 g of crude product, which was purified by column chromatography on silica gel to give 500 mg of pure product (11F).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08969373B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-8de8db36e93743beac580d3ea7b1ab47 |
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| Source note | uspto-grants-2015_03 |
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