Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | 1-Chloro-4,5-difluoro-2-nitrobenzene | HCID 10130330 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10945160 | HCID 10945160 | 95% |
Reaction Steps
A solution of 19.3 g (0.08 mol) of 2-chloro-4,5-difluoronitrobenzene in 100 g of toluene are introduced into a 200 ml three-necked flask fitted with dropping funnel, precision-ground glass stirrer and reflux condenser. 18.1 g (0.21 mol) of piperazine are added dropwise to this solution at room temperature and with stirring over the course of one hour. The mixture is then stirred at room temperature for a further 2 hours. The reaction solution formed during the reaction is washed three times with 20 ml of water in each case and dried. The solvent is removed to give 18.5 g (0.071 mmol) of 2-chloro-5-fluoro-4-piperazinonitrobenzene. This corresponds to a yield of 95%, based on 2-chloro-4,5-difluoronitrobenzene used. 2-Chloro-5-fluoro-4-piperazinonitrobenzene of the following formula ##STR5## has a melting point of 91.5° C. (purity: 92.9%, determined by HPLC).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05917037 |
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| Source dataset | uspto-grants-1999_06 |
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| ORD ID | ord-624d4f850f0b4ad5900890cf173bb01e |
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| Source note | uspto-grants-1999_06 |
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