HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethyl Sulfoxide → 6-Chloro-N-methyl-N-(tetrahydro-2H-pyran-4-ylmethyl)-2-pyrazinamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethyl Sulfoxide | HCID 679 | — |
| Edukt | 2,6-Dichloropyrazine | HCID 78504 | — |
| Edukt | Tetrahydro-N-methyl-2H-pyran-4-methanamine | HCID 22225668 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 6-Chloro-N-methyl-N-(tetrahydro-2H-pyran-4-ylmethyl)-2-pyrazinamine | HCID 53410302 | 98,3% |
Reaktionsbedingungen
| Temperatur | 70 °C |
|---|
Reaktionsschritte
A mixture of 2,6-dichloropyrazine (298 mg, 2.000 mmol), DMSO (6 ml), TEA (0.418 ml, 3.00 mmol) and N-methyl-1-(tetrahydro-2H-pyran-4-yl)methanamine (264 mg, 2.040 mmol) was stirred at 70° C. for 16 hours, and the reaction progress was followed by LCMS. The crude reaction mixture was let cool to room temperature, diluted with 150 ml of ethyl acetate, washed with 1M NaOH soln. (1×), water (2×), saturated salt soln. (1×), dried with sodium sulfate, filtered, and concentrated to constant mass, giving 475 mg of the title compound as free base, which was used without further purification. LCMS (m/z): 242.0 (MH+), retention time=0.85 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08778951B2 |
| Quelldatensatz | uspto-grants-2014_07 |
| ORD ID | ord-d65309e6f5754b1f8a9071880b3fd604 |
| Quellennotiz | uspto-grants-2014_07 |