HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclopropanemethanol → 2-(4-Chloro-phenyl)-3-cyclopropylmethoxy-pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclopropanemethanol | HCID 75644 | — |
| Reactant | 2-(4-Chloro-phenyl)-3-fluoro-pyridine | HCID 66678603 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 2-(4-Chloro-phenyl)-3-cyclopropylmethoxy-pyridine | HCID 66678697 | 74.9% |
Reaction Steps
To a mixture of 16.20 g cyclopropanmethanol in 150 ml dry DMSO 11 g sodium hydride (55%) was added and the mixture was stirred at room temperature for 30 minutes. A solution containing 37.30 g 2-(4-chloro-phenyl)-3-fluoro-pyridine in 50 mL dry DMSO was added dropwise. The reaction mixture was then stirred at room temperature for 3 h. The resulting suspension was partitioned between water and methylene chloride, the phases were separated. The organic phase was washed with brine; then dried over MgSO4 and purified by chromatography on silica gel with a gradient of heptane to heptane:ethylacetate=2:1 to yield 34.95 g (74.90%) of the title compound as yellow oil, MS 260.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08729105B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-5e7d7c8529a848e9ab8a73de06b8eb5c |
| Source note | uspto-grants-2014_05 |