HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium periodate → HCID 178432825, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium periodate | HCID 23667635 | — |
| Reactant | HCID 178503299 | HCID 178503299 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178432825 | HCID 178432825 | — |
Reaction Steps
0.87 g (2.3 mmol) of 5-hydroxy-2-methyl-2-methylsulfanyl-4-(2-methyl-6-trifluoromethylpyridine-3-carbonyl)bicyclo[4.1.0]hept-4-en-3-one (Compound A2-D113), dissolved in 8 ml of methanol, is warmed for 3 hours at a temperature of 50° C. in the presence of 0.56 g of sodium periodate. The mixture is then partitioned between ethyl acetate an d sodium chloride solution, concentrated, and the crude product is purified by chromatography (mobile phase: ethyl acetate/m ethanol 19:1). Pure 5-hydroxy-2-methanesulfinyl-2-methyl-4-(2-methyl-6-trifluoromethylpyridine-3-carbonyl)bicyclo[4.1.0]hept-4-en-3-one is obtained as tautomer and isomer mixture of melting point 159.5-160° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06534445B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-378bdd8b893943338db42c6fb3df506b |
| Source note | uspto-grants-2003_03 |