Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | 1-Fluoro-3-nitrobenzene | HCID 9823 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 1-(3-Nitrophenyl)piperazine | HCID 2760216 | 71% |
Reaction Steps
A suspension of 3-fluoronitrobenzene (23 ml; 0.21 mol) and piperazine (55.5 g; 0.64 mol) in anhydrous NMP (30 ml) was heated to 70° C. for five days. The cooled mixture was diluted with water (250 ml) and extracted with dichloromethane. The combined extracts were dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by column-chromatography on silica gel eluting subsequently with mixtures of ethyl acetate and methanol (4:1 v/v) and (1:1 v/v) to leave the desired product as oily crystals (30.7 g; 71%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06936613B2 |
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| Source dataset | uspto-grants-2005_08 |
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| ORD ID | ord-0b908b89a1d74021a3ed1d0557b57d7f |
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| Source note | uspto-grants-2005_08 |
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