Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bicarbonate Ion | HCID 769 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 86602965 | HCID 86602965 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11587886 | HCID 11587886 | — |
Reaction Steps
To 11 ml of THF cooled to 0° C. were added 0.26 g of Potassium tert-butylate and 20 μl of water. Then a solution of 0.40 g 3-Chloro-2-(2-chloro-pyridin-4-yl)-3-[5-(4-fluoro-phenyl)-1,4-dimethyl-1H-pyrazol-3-yl]-propenal in 7 ml of THF was added at 0°. After stirring for 1 h at 5° C., 10 ml of 5% Bicarbonate solution were added and the aqueous phase was extracted twice with Ethyl acetate. The combined organic phases were washed with water and brine, dried over magnesium sulfate, filtered and evaporated. The crude product (0.28 g, yellow oil) was purified by chromatography on silica gel (Heptane/Ethyl acetate 4:1). The desired product was obtained as a white solid (0.275 g, 82%), MS: m/e=326.0 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08293916B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-bf745c8c437c412ca3377726204fb88f |
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| Source note | uspto-grants-2012_10 |
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