HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triacetoxyperiodinane → HCID 66618805, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | HCID 66629741 | HCID 66629741 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66618805 | HCID 66618805 | 22.5% |
Reaction Steps
2-[6-Methoxy-5-(4-methylimidazol-1-yl)pyridin-2-yl]-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro[1,2,4]triazolo[1,5-a]pyridin-6-ol obtained in Example 26 (125 mg) was dissolved in methylene chloride (3 mL), and Dess-Martin reagent (226 mg) was added at room temperature. After stirring for 30 minutes, the reaction solution was partitioned with a saturated sodium bicarbonate solution and ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and then concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (mobile phase:ethyl acetate/heptane=0 to 100%→methanol/ethyl acetate=10%) to obtain the title compound (28 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08754100B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-8232c7a0c69f439d9a40ca7f63360975 |
| Source note | uspto-grants-2014_06 |