Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzyl Alcohol | HCID 244 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Methyl 5-hydroxypyridine-3-carboxylate | HCID 354317 | — |
| Reactant | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57421820 | HCID 57421820 | — |
Reaction Steps
0.31 g (2 mmol) of 5-hydroxy-nicotinic acid methyl ester and 3.1 g (4 mmol) of polymer-supported triphenylphosphine were combined in a flask charged with 45 mL of THF and 0.31 mL (3 mmol) of benzyl alcohol, and shaken at r.t. until the starting materials dissolved. The reaction mixture was then cooled to 0° C. with a water/brine bath, 0.58 mL (3 mmol) of DIAD was added and the reaction slurry then stirred overnight at r.t. The reaction mixture was filtered and the resin was washed 3 times with DCM/MeOH=1:1. The organic layer was then evaporated and flashed (EtOAc/hexanes=1:2) to give the desired 5-benzyloxy-nicotinic acid methyl ester, which was subsequently hydrolyzed according to general procedure B to give 5-benzyloxy-nicotinic acid which was used in the next step without further purification. LCMS: 230 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08598353B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-b679ca6654f147ff98e48adc914e57a3 |
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| Source note | uspto-grants-2013_12 |
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