HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propiolic Acid → HCID 22258165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propiolic Acid | HCID 10110 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 22258173 | HCID 22258173 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22258165 | HCID 22258165 | — |
Reaction Steps
126.8 mg (0.78 mmol) of 1-(1H-imidazol-1-ylcarbonyl)-1H-imidazole and 45.5 mg (0.65 mmol) of propiolic acid are dissolved in 8 ml THF. The mixture is stirred for 3 h at rt. To this solution 131.7 mg (0.43 mmol) of 1-(2,4-Difluorophenyl)-2-(4,6-dimethyl-4,5,6,7-tetrahydro-1H-benzimidazol-2-yl)ethanone (example X) are added and the mixture is stirred for 20 h at rt. The solvent is evaporated under vacuum and the crude is purified over preparative HPLC (RP18-column, eluent: acetonitrile-water-gradient. The isomers are isolated after purification over preparative HPLC (Daicel Chiralpak AD, eluent: iso-hexane-ethanol v/v 30:70):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06984646B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-f7e3cea6d4d44a81ab3b3e4b0d4b447c |
| Source note | uspto-grants-2006_01 |