HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 3-(Difluoromethoxy)-2-methoxypyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | 2-Chloro-3-(difluoromethoxy)pyridine | HCID 53302035 | — |
| Product | 3-(Difluoromethoxy)-2-methoxypyridine | HCID 66617382 | 56% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
As shown in step 3-ii of Scheme 3, an excess of sodium metal was dissolved into 20 mL anhydrous methanol and 2-chloro-3-(difluoromethoxy)pyridine (2.0 g, 11.1 mmol) in anhydrous methanol was added. The reaction mixture was stirred in a sealed vessel at 100° C. for 6 hours. The volatiles were removed under reduced pressure and the residue was partitioned between EtOAc and brine. The brine was extracted with EtOAc and the combined organics were dried over Na2SO4, filtered, and the volatiles removed under reduced pressure. The product was purified by silica gel chromatography (DCM) to yield 3-(difluoromethoxy)-2-methoxypyridine as a colorless oil (Compound 1007, 1.1 g, 56% yield: ESMS (M+H) 176.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524906B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-b5a18a3ea26b4392a1df569370a60993 |
| Source note | uspto-grants-2013_09 |