HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(3-Cyano-5-fluorophenyl)-4-(2,2,2-trichloroethoxycarbonyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | HCID 18545236 | HCID 18545236 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(3-Cyano-5-fluorophenyl)-4-(2,2,2-trichloroethoxycarbonyl)piperazine | HCID 18545413 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
In 30 ml of dichloromethane was suspended 2.54 g of 1-(3-cyano-5-fluorophenyl)piperazine hydrochloride, and the suspension was cooled to 0° C. To the suspension were added 7.3 ml of triethylamine and 3 ml of 2,2,2-trichloroethyl chloroformate, followed by stirring at room temperature for 2 hours. The reaction mixture was washed with water and then with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was subjected to silica gel column chromatography using chloroform as a developing solvent. The fraction containing the desired compound was concentrated to give 4.79 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06169086A |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-e5095b7dc2d94991b3062272bac7517e |
| Source note | uspto-grants-2001_01 |