HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → HCID 14793344, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Bromine | HCID 24408 | — |
| Edukt | ethyl 3-(tert-butyl)-1-methyl-1H-pyrazole-5-carboxylate | HCID 2799344 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 14793344 | HCID 14793344 | — |
Reaktionsschritte
To a mixture of 5-tert-butyl-2-methyl-pyrazole-3-carboxylic acid ethyl ester (2.00 g, 9.51 mmol) and K2CO3 (3.94 g, 28.5 mmol) in DCM (120 mL), in the dark, was added Br2 (1.46 mL, 28.5 mmol) slowly under Ar. After stirring at room temperature for 3 h under Ar, the resulting mixture was quenched with saturated aqueous Na2S2O3 (50 mL). The organic layer was separated and washed with H2O (50 mL) and brine (50 mL), then dried with Na2SO4. Removal of the solvent under reduced pressure yielded a white solid. 1H-NMR (400 MHz, CDCl3) δ: 4.40 (q, J=7.1 Hz, 2H), 4.08 (s, 3H), 1.43 (t, J=7.1 Hz, 3H), 1.42 (m, 9H). Mass Spectrum (LCMS, ESI pos.) Calculated For C11H17BrN2O2: 289.1 (M+H), Measured: 289.1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09023846B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-6068e5464a65454e84925cd59103ee60 |
| Quellennotiz | uspto-grants-2015_05 |