HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → Methyl 2-(6-chloro-5-fluoropyridin-3-yloxy)-4-fluorobenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methyl 2,4-Difluorobenzoate | HCID 2782897 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | 2-Chloro-3-fluoro-5-hydroxypyridine | HCID 40424737 | — |
| Solvent | 2-Methyltetrahydrofuran | HCID 7301 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methyl 2-(6-chloro-5-fluoropyridin-3-yloxy)-4-fluorobenzoate | HCID 86642876 | — |
Reaction Steps
To a solution of 6-chloro-5-fluoropyridin-3-ol (0.977 g) in 2-methyltetrahydrofuran (12 mL) was added potassium 2-methylpropan-2-olate (1.0M in tetrahydrofuran, 7.28 mL). After stirring for 15 minutes at room temperature, methyl 2,4-difluorobenzoate (1.710 g) was added as a solution in 2-methyltetrahydrofuran (2 mL) followed by N,N-dimethylformamide (2 mL) then the reaction was heated to 75° C. under a nitrogen atmosphere. After stirring overnight the reaction was cooled, diluted with ethyl acetate (100 mL) and washed with water (50 mL) and brine (50 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography (GraceResolv 40 g) eluting with a gradient of 2% to 15% ethyl acetate/hexanes gave the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557983B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-206fc5527243427f862685460c7e2b48 |
| Source note | uspto-grants-2013_10 |