HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 5-(2,2,3,3-Tetrafluoro-propoxy)-pyridine-2-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,2,3,3-Tetrafluoropropyl trifluoromethanesulfonate | HCID 3792475 | — |
| Reactant | Methyl 5-hydroxypyridine-2-carboxylate | HCID 4715126 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 5-(2,2,3,3-Tetrafluoro-propoxy)-pyridine-2-carboxylic acid methyl ester | HCID 57475874 | — |
Reaction Steps
A solution of 5-hydroxy-pyridine-2-carboxylic acid methyl ester (2.0 g, 13.1 mmol) in acetone (40 ml) was treated with potassium carbonate (5.415 g, 39.2 mmol) and trifluoro-methanesulphonic acid 2,2,3,3-tetrafluoropropyl ester. After 4 hours stirring at room temperature the suspension was diluted with diethylether. After filtration the solution was evaporated and the yellow solid purified by chromatography on silica gel using a gradient of heptane/ethyl acetate=100:0 to 30:70 as the eluent. The 5-(2,2,3,3-tetrafluoro-propoxy)-pyridine-2-carboxylic acid methyl ester was obtained as a light yellow solid (3.49 g, 76% of theory). MS (ISP): m/z=468.1 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115098B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-d72cc5c8fc6246a7b01a97109b9eb489 |
| Source note | uspto-grants-2015_08 |