Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 3-Hydroxypyridine | HCID 7971 | — |
| Reactant | Ethanol, 1-ethoxy-2,2,2-trifluoro- | HCID 9897 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10488012 | HCID 10488012 | 19.2% |
Reaction Steps
Potassium carbonate (4.66 g, 36.3 mmol) was added to the mixture of pyridin-3-ol (2.00 g, 21.0 mmol) and 1-ethoxy-2,2,2-trifluoroethanol (3.30 g, 23.1 mmol), and the mixture was stirred for 4 hours at 100° C. under nitrogen atmosphere. This reaction solution was cooled to room temperature, followed by adding water and ethyl acetate to the reaction solution, washing the organic layer with a saturated saline solution, drying the layer with anhydrous sodium sulfate, and thereafter concentration under reduced pressure. The obtained residue was purified by silica gel column chromatography (Purif-Pack SI200, hexane:ethyl acetate:=40:60) to obtain the title compound (780 mg, yield: 19%) as a white amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08609699B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-5bff0dc5626b45bf9321299709c1e7f4 |
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| Source note | uspto-grants-2013_12 |
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