HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118431899, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,4-Difluorophenylhydrazine hydrochloride | HCID 2733301 | — |
| Reactant | HCID 131735938 | HCID 131735938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 118431899 | HCID 118431899 | 95.3% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
1-(3-Bromo-phenyl)-4,4,5,5,5-pentafluoro-pent-1-en-3-one (1.8 g, 5.3 mmol) prepared in Step 1, 2,4-difluorophenylhydrazine hydrochloride (1.2 g, 6.4 mmol) and conc. hydrochloric acid (100.0 uL) were added to ethanol (15.0 mL). The reaction mixture was stirred at 100° C. for 8 hours, quenched with a saturated solution of sodium hydrogen carbonate, and then extracted with ethyl acetate three times. The combined extract was washed with brine, dried on anhydrous magnesium sulfate, and then concentrated under reduced pressure to give a yellow liquid residue. The resulting residue was purified by silica gel column chromatography (eluent: ethyl acetate/n-hexane=1/60) to give 2.3 g of the titled compound as a yellow liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376420B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-b17e553b1bd740a682acd035525e8deb |
| Source note | uspto-grants-2016_06 |