HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Phenylpiperazine → HCID 67167457, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Phenylpiperazine | HCID 7096 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 67167457 | HCID 67167457 | 96.33% |
Reaction Steps
50 ml of ethyl acetate, 13.5 ml of 4-phenyl piperazine, and 15.30 ml of diisopropyl ethyl amine were added into a 250 ml triple-neck flask. After magnetic stirring at room temperature, 9.0 ml of 3,4-difluoro-nitrobenzene was added. The reaction was carried out for 105 hours, followed by extraction with 150 ml of ethyl acetate for three times (150 ml×3). The extract was washed three times with saturated NaCl solution (150 ml×3), dried with anhydrous magnesium sulfate (MgSO4), and evaporated to dryness. An orange yellow solid was obtained which was recrystallized with a mixture of acetone and water in volumetric ratio of 9:1 to produce orange yellow crystals (23.66 g) with a yield of 96.33%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916567B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-08522411f986470189ff0a17e5ca754d |
| Source note | uspto-grants-2014_12 |