HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → 5-(2-Methoxyethyl)-2-nitro-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | 2-Methoxyethylamine | HCID 8018 | — |
| Reactant | 1-(2-Bromoethyl)-5-(chloromethyl)-3-nitro-1H-pyrazole | HCID 86684540 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5-(2-Methoxyethyl)-2-nitro-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrazine | HCID 86683990 | 75.1% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A microwave vial equipped with a magnetic stirrer was charged with 296c (2.67 g, 10.0 mmol), 2-methoxyethanamine (2.25 g, 30.0 mmol), and DMSO (14 mL). The reaction mixture was heated at 120° C. under microwave irradiation for 1.0 h. It was cooled to room temperature and diluted with ethyl acetate (40 mL). The mixture was washed with water (3×15 mL). The organic layer was dried and filtered. The filtrate was concentrated under pressure and the residual was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 296d (1.7 g, 75%) as a yellow solid. MS-ESI: [M+H]+ 227.0
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08716274B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-148d31736d3744a2838614602024ca64 |
| Source note | uspto-grants-2014_05 |