HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-1-fluoro-4-nitrobenzene → 1-acetyl-4-(2-chloro-4-nitrophenyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-1-fluoro-4-nitrobenzene | HCID 67688 | — |
| Reactant | 1-Acetylpiperazine | HCID 83795 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-acetyl-4-(2-chloro-4-nitrophenyl)piperazine | HCID 2887588 | — |
Reaction Steps
2-Chloro-1-fluoro-4-nitrobenzene (10 g, 57 mmol) and 1-acetylpiperazine (14.6 g, 114 mmol) were heated neat at 55° C. for 1 h. Then the reaction mixture was allowed to cool down to room temperature. The viscous orange solution was diluted with EtOAc and water. The organics were washed with water (3 times), brine, dried and evaporation of the solvent gave an orange oil which was triturated with isohexane. After evaporation of solvent the title compound was obtained as a yellow solid which was dried overnight in vac oven at 50° C. (15.68 g, 97%). It was used without further purification. NMR (400 MHz) 2.03 (d, 3H), 3.18 (dt, 4H), 3.62 (m, 4H), 7.30 (d, 1H), 8.17 (dd, 1H), 8.26 (d, 1H); m/z 284-286.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07655652B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-b04e436f1cae4cdaa086f793015682a1 |
| Source note | uspto-grants-2010_02 |