HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 66628239, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Isobutyl iodide | HCID 10556 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | HCID 70223867 | HCID 70223867 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66628239 | HCID 66628239 | — |
Reaction Steps
Potassium carbonate (15.7 mg, 113 μmol, 2.1 eq.), 18-crown-6 (30 mg, 113 μmol, 2.1 eq.) and 1-iodo-2-methylpropane (21 mg, 113 μmol, 2.1 eq.) were added to a solution of benzyl {(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}carbamate (30 mg, 54 μmol) in DMF (2 ml). The reaction mixture was stirred at RT for 12 h and then concentrated under reduced pressure. The residue was acidified with acetic acid (3 eq.) and then purified by preparative HPLC (Kromasil C18 column, 5 μm, 50×20 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (25 mg, 76% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359362B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-b849bd956412490ca8cc4c2a09391ff8 |
| Source note | uspto-grants-2016_06 |