HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → 2-Fluoro-4-iodo-5-[2-[(tetrahydro-2H-pyran-2-yl)oxy]ethoxy]pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-(2-Bromoethoxy)tetrahydro-2H-pyran | HCID 86621 | — |
| Reactant | 6-Fluoro-4-iodopyridin-3-ol | HCID 66674592 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 2-Fluoro-4-iodo-5-[2-[(tetrahydro-2H-pyran-2-yl)oxy]ethoxy]pyridine | HCID 66738444 | 75.6% |
Reaction Steps
Add 6-fluoro-4-iodo-pyridin-3-ol (0.5 g, 2.09 mmol) to a suspension of sodium hydride (60% dispersion in mineral oil, 0.1 g, 2.51 mmol) in DMF (6 mL). Stir the mixture for 1 h. Add 2-(2-bromo-ethoxy)-tetrahydropyran (0.51 g, 2.34 mmol). Stir the solution at RT overnight. Dilute the mixture with ethyl acetate and water. Wash the organic layer with aqueous saturated sodium chloride and water. Dry the mixture over sodium sulfate. Concentrate the solution in vacuo. Purify by column chromatography (10% ethyl acetate in hexane) to afford the title compound (0.58 g, 75.5%) as a light yellow oil. MS (ES) m/z 368 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08114872B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-0a17f13cd06b4b2995fa362237b964c9 |
| Source note | uspto-grants-2012_02 |