HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 2-(4-Bromo-benzyloxy)-5-methyl-pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 4-Bromobenzyl alcohol | HCID 70119 | — |
| Edukt | 2-Fluoro-5-methylpyridine | HCID 2774635 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 2-(4-Bromo-benzyloxy)-5-methyl-pyridine | HCID 59255449 | 59,3% |
Reaktionsschritte
To an N,N-dimethylformamide (50.0 mL) solution of 4-bromobenzyl alcohol (4.54 g, 24.3 mmol) was added sodium hydride (1.00 g, 25.0 mmol, 60% in oil) under nitrogen atmosphere at 0° C., which was stirred for 30 minutes at room temperature. 2-Fluoro-5-methylpyridine (1.80 g, 16.2 mmol) was then added at 0° C., and stirred for 5 hours at room temperature. Water was added to the reaction solution at room temperature, which was then extracted with ethyl acetate. The organic layer was separated and 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=1:15) to obtain the title compound (2.67 g, 59.3%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08841327B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-facb86b0ae294aae8f86b7ad66b231a8 |
| Quellennotiz | uspto-grants-2014_09 |