HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 764809, compound → HCID 13544863, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 764809 | HCID 764809 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 13544863 | HCID 13544863 | 66.3% |
Reaction Steps
To a suspension of 1-(4-fluorophenyl)-4-[ (4-nitrophenyl)methyl ]piperazine (1.5 g, 0.005 M) in 15 ml of anhydrous ether is added dropwise a solution of 15 ml of titanium trichloride in water (20% solution in water), under nitrogen at room temperature. After complete addition, the mixture is quenched with 10% ammonium hydroxide solution and extracted with methylene chloride. The methylene chloride solution is washed with water, dried (anhydrous sodium sulfate), and concentrated to a yellow solid. This, after recrystallization from ethyl acetate/Skellysolve® B, gives 900 mg (64%) of white crystalline 1-[ (4-aminophenyl)methyl ]-4-(4-fluorophenyl)piperazine of melting point 130° - 132° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04140775 |
| Source dataset | uspto-grants-1979_02 |
| ORD ID | ord-3b834d0dba7c445a9f61cf71ae4dfa70 |
| Source note | uspto-grants-1979_02 |