HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 2-(4-Chloro-3-difluoromethoxy-2-pyridyl)-2-cyclopropylethanal
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 2-(4-Chloro-3-difluoromethoxy-2-pyridyl)-2-cyclopropyl-1-methoxyethene | HCID 86586470 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(4-Chloro-3-difluoromethoxy-2-pyridyl)-2-cyclopropylethanal | HCID 18629323 | 56.7% |
Reaction Steps
130 mg of 2-(4-chloro-3-difluoromethyl-2-pyridyl)-2-cyclopropyl-1-methoxyethene (XI) was dissolved in 10 ml of THF, which was added 3 ml of dilute sulfuric acid and concentrated at 50° C. under reduced pressure. The resulting mixture was poured into water and neutralized with saturated sodium bicarbonate solution, and thereafter, extracted with chloroform. The resulting organic layer was washed with saturated salt water, and thereafter, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; hexane:ethyl acetate=4:1) to obtain 70 mg of 2-(4-chloro-3-difluoromethyl-2-pyridyl)-2-cyclopropylethanal (XII).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06525066B2 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-6b18edbb1dd74d8ab28c971c0da11d64 |
| Source note | uspto-grants-2003_02 |