Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-Chloroethyl methyl carbonate | HCID 13506641 | — |
| Edukt | HCID 178496175 | HCID 178496175 | — |
| Katalysator | Tetrabutylammonium Bromide | HCID 74236 | — |
| Lösungsmittel | Methyl Ethyl Ketone | HCID 6569 | — |
| Produkt | HCID 66884422 | HCID 66884422 | 52,6% |
Reaktionsschritte
5-Hydroxy-1,3-dimethylpyrazol-4-yl 3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)phenyl ketone (300 mg) was dissolved in 2-butanone (10 mL), and potassium carbonate (130 mg) and tetrabutyl ammonium bromide (15 mg) were added. After stirring at room temperature for 10 minutes, 1-chloroethyl methyl carbonate (purity: 85%, 270 mg) was added at room temperature, followed by heating and refluxing for 3 hours. After completion of the reaction, the reaction solution was cooled to room temperature and poured into water and then extracted with ethyl acetate. The organic layer was washed with a 1N hydrochloric solution and a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The obtained residue was purified by column chromatography (n-hexane:ethyl acetate=1:1) to obtain the desired product (200 mg) as slightly yellow solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08466089B2 |
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| Quelldatensatz | uspto-grants-2013_06 |
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| ORD ID | ord-e222511c5c7342a9a53fd44aa05d9c93 |
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| Quellennotiz | uspto-grants-2013_06 |
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