HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trifluoroethanol → HCID 68014918, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 89586363 | HCID 89586363 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68014918 | HCID 68014918 | 54.4% |
Reaction Steps
To a solution of 2,2,2-trifluoroethanol (48 mg) in DMF (1 mL) was added 60% NaH (19.2 mg) under ice-cooling. The reaction mixture was stirred at room temperature for 30 min, and 1-[2-fluoro-4-(1H-pyrazol-1-yl)phenyl]-3-(1-phenyl-1H-pyrazol-5-yl)furo[3,2-c]pyridazin-4(1H)-one (70 mg) was added. The reaction mixture was stirred at 100° C. for 6 hr, and saturated aqueous sodium hydrogen carbonate solution was added. The reaction mixture was extracted with ethyl acetate, the extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (45 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150588B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-ff1ac76a145740c3ad97fe3fc4a82127 |
| Source note | uspto-grants-2015_10 |