Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hexane | HCID 8058 | — |
| Edukt | Ethyl trifluoroacetate | HCID 9794 | — |
| Edukt | 3-(2,5-dimethyl-1H-pyrrol-1-yl)-1-methyl-1H-pyrazole | HCID 13248995 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 59394508 | HCID 59394508 | — |
Reaktionsschritte
To a solution of 3-(2,5-dimethyl-pyrrol-1-yl)-1-methyl-1H-pyrazole (1.5 g, 8.6 mmol) in THF (100 mL) at −78° C., 2.5M nBuLi in Hexane (4.1 mL, 10.3 mmol) is added and stirred for 1.5 hours followed by the addition of trifluoro-acetic acid ethyl ester (1.5 g, 10.3 mmol). After 10 min the ice bath is removed and the reaction is allowed to reach room temperature. Then the reaction is cooled down to −78° C. again and methylmagnesium bromide (1.0 M solution in hexane, 8.6 mL) is added. After 5 min the ice bath is removed and the mixture is stirred at room temperature for 3 hour, poured into water, separated, and the water layer is extracted with DCM. The organic layers are combined and concentrated. The residue is purified by FCC to give the title compound. MS (ESI) m/z 288.1 (M+1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08541432B2 |
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| Quelldatensatz | uspto-grants-2013_09 |
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| ORD ID | ord-481c7e95d52345e5a01614e6bb39f2fd |
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| Quellennotiz | uspto-grants-2013_09 |
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