HuagongsheHuagongshe Chemistry Print Report · For research reference only
(2,3,4-Trimethoxy-6-methylphenyl)(2,5-dichloro-3-trifluoromethyl-4-pyridyl)methanol → 2,3,4-Trimethoxy-6-methylbenzoyl-2,5-dichloro-3-trifluoromethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (2,3,4-Trimethoxy-6-methylphenyl)(2,5-dichloro-3-trifluoromethyl-4-pyridyl)methanol | HCID 12151535 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2,3,4-Trimethoxy-6-methylbenzoyl-2,5-dichloro-3-trifluoromethylpyridine | HCID 12151536 | 89.1% |
Reaction Steps
14 g of manganese dioxide was added to a solution having 3.5 g (8.2 mmol) of (2,3,4-trimethoxy-6-methylphenyl)(2,5-dichloro-3-trifluoromethyl-4-pyridyl)methanol obtained in Step (b) dissolved in 100 ml of toluene, followed by stirring under reflux with heating for 6 hours. The mixture was cooled and then subjected to filtration, and toluene was distilled off under reduced pressure. The crude product was purified by silica gel column chromatography to obtain 3.1 g (yield: 89%) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-2,5-dichloro-3-trifluoromethylpyridine (melting point 106 to 109° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653277B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-b534166b2efb4ec29854c330a2bbc2a3 |
| Source note | uspto-grants-2014_02 |