HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloromethyl Methyl Ether → 2-Bromo-5-(methoxymethoxy)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-Bromo-5-hydroxypyridine | HCID 2762865 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Bromo-5-(methoxymethoxy)pyridine | HCID 57433666 | — |
Reaction Steps
To a solution of 6-bromopyridin-3-ol (25 g, 144 mmol) in DMF (300 mL) at 0° C. under N2 is added portionwise NaH (5.7 g, 144 mmol) over 5 min. The reaction was stirred 1 h, then chloro(methoxy)methane (12 g, 144 mmol) was added and the reaction stirred an additional 1 h at 0° C. Saturated sodium bicarbonate (500 mL) was added slowly and the suspension stirred 30 min and warmed to rt. The solution was extracted with EtOAc (3×400 mL), the combined organic layers washed with H2O (500 mL), saturated NaCl (500 mL), dried (Na2SO4), and concentrated in vacuo to give the title compound as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07973047B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-7e6ee0ae993f4209b6cb461513c40d58 |
| Source note | uspto-grants-2011_07 |