HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 118431956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 118431866 | HCID 118431866 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 118431956 | HCID 118431956 | 39.4% |
Reaction Steps
1-(2,4-Difluoro-phenyl)-5-[5-(piperazin-1-yl)-thiophen-2-yl]-3-pentafluoroethyl-4,5-dihydro-1H-pyrazole hydrochloride (30.0 mg, 0.07 mmol) prepared in Step 1, triethylamine (47.0 uL, 0.34 mmol) and methanesulfonyl chloride (11.6 mg, 0.10 mmol) were added to dichloromethane (1.0 mL). The reaction mixture was stirred at room temperature for 18 hours, washed with distilled water, 1N hydrochloride, a saturated solution of sodium hydrogen carbonate, and 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=2/1) to give 15.0 mg 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-e0ddee8a0fc24bab8a60da17dc9095ba |
| Source note | uspto-grants-2016_06 |