Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 68720433 | HCID 68720433 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 68720410 | HCID 68720410 | — |
Reaction Steps
To a solution of Example 7A (0.106 g, 0.344 mmol) in a solvent mixture of methanol (2 mL) and acetic acid (2 mL) was added Zn powder (0.067 g, 1.03 mmol). The reaction was heated to 50° C. for 5 h, and was then cooled to room temperature. The reaction was quenched by the addition of saturated aqueous NaHCO3 (5 mL) and ethyl acetate (5 mL). The layers were separated, and the aqueous was extracted with additional ethyl acetate (2×5 mL). The combined organics were dried with anhydrous Na2SO4, filtered, and concentrated under reduced pressure to yield the title compound which was used without further purification. MS (ESI) m/z 278 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08901152B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-45b76adc725946fb9e1a27b3167d7059 |
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| Source note | uspto-grants-2014_12 |
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