HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86701834, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Carbamimidic acid, methyl ester, sulfate (1:1) | HCID 169039 | — |
| Reactant | HCID 86701841 | HCID 86701841 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86701834 | HCID 86701834 | 62% |
Reaction Steps
To a solution of ethyl (7E)-7-[(dimethylamino)methylidene]-N-methoxy-N,1-dimethyl-8-oxo-1,4,5,6,7,8-hexahydrocyclohepta[c]pyrazole-3-carboxamide (1.62 g, 5.3 mmol) in CH3CN (130 ml), O-methylisourea sulphate (5.22 g, 21.2 mmol) and K2CO3 (3 g, 22.2 mmol) were added. The reaction mixture was stirred at reflux for 16 h, then it was filtered to remove salts and the solvent was evaporated. The residue was suspended in DCM and washed with water; the organic phase was dried on Na2SO4, filtered and concentrated. The crude was purified by flash-chromatography in silica gel (hexane/AcOEt:1/1) to afford 1 g (62% yield) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916577B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-0f86b1caf1c949d5873082161cbe389a |
| Source note | uspto-grants-2014_12 |