Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | 3-(Diethylamino)pyrrolidine | HCID 19961995 | — |
| Edukt | HCID 178489782 | HCID 178489782 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178463849 | HCID 178463849 | 82% |
Reaktionsschritte
N,N-diethylpyrrolidin-3-amine (142 mg, 1.00 mmol) was added to 5-chloro-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (136 mg, 0.35 mmol) in anhydrous dimethylsulfoxide (1.75 ml) at 25° C. The resulting solution was stirred at room temperature for 50 mins. The reaction mixture was diluted with methanol (5.00 ml) and the crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 7M NH3/MeOH and fractions were evaporated to dryness to afford impure product as a brown dry film. The crude product was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the title compound (141 mg, 82%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07737149B2 |
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| Quelldatensatz | uspto-grants-2010_06 |
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| ORD ID | ord-a898c3233bb74110a0dfb2eb5db2b762 |
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| Quellennotiz | uspto-grants-2010_06 |
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