HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 3-Fluoro-4-(pyridin-2-ylmethoxy)-benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Piconol | HCID 11474 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,4-Difluorobenzaldehyde | HCID 588088 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-Fluoro-4-(pyridin-2-ylmethoxy)-benzaldehyde | HCID 59255224 | 45.6% |
Reaction Steps
To an N,N-dimethylformamide (40.0 mL) solution of 2-(hydroxymethyl)-pyridine (3.00 g, 27.5 mmol) was added sodium hydride (1.00 g, 25.0 mmol, 60% in oil) under nitrogen atmosphere at 0° C., which was stirred for 20 minutes at room temperature. 3,4-Difluorobenzaldehyde (4.69 g, 33.0 mmol) was then added at 0° C., and stirred for 20 minutes at room temperature. Water was added to the reaction solution at room temperature, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:1→2:1) to obtain the title compound (2.90 g, 45.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841327B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-3eb2895945b5409e948905dc8beac549 |
| Source note | uspto-grants-2014_09 |