HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 1-(3-Fluoro-4-trifluoromethyl-phenyl)-piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 4-(3-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 59793628 | — |
| Solvent | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Product | 1-(3-Fluoro-4-trifluoromethyl-phenyl)-piperazine | HCID 59793595 | 78% |
Reaction Steps
4-(3-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (853 mg, 2.45 mmol) was stirred in a mixture of trifluoroacetic acid/dichloromethane (5 mL, 25% v/v) for 20 min at room temperature. The reaction mixture was combined with 25 mL of CH2Cl2 and was washed with sat'd NaHCO3 (2×10 mL) and brine. The resulting CH2Cl2 layer was dried over anhydrous Na2SO4 and was concentrated to yield crude amine. The product was further purified by silica gel chromatography (gradient eluent 0-10% MeOH in dichloromethane) to provide 4-(3-fluoro-4-trifluoromethyl-phenyl)-piperazine (473 mg, 78%). The product was used directly in step 3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517884B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-8f33f4eea72443b0a65a1195ca8a5195 |
| Source note | uspto-grants-2009_04 |