Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Chloro-2-nitroaniline | HCID 74218 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10013146 | HCID 10013146 | — |
Reaction Steps
240 mmol of imidazole, 240 mmol of 2-amino4-chloronitrobenzene and 240 mmol of potassium carbonate in 450 ml of dimethylformamide (DMF) are stirred in a 1 litre round-bottomed flask. The mixture is maintained at 130° C. with stirring for 48 hours. After the DMF has been removed by evaporation, the residue is taken up in water. The precipitate that forms is filtered off and then washed with water. It is then dissolved in 550 ml of 1N hydrochloric acid. After insoluble material has been filtered off, the filtrate is rendered alkaline and the precipitate that forms is filtered off and washed with water. After drying, the expected product is obtained after purification by chromatography on silica gel using a dichloromethane/methanol mixture(95/5).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06040327 |
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| Source dataset | uspto-grants-2000_03 |
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| ORD ID | ord-2849616f59764d5fa05b26f6ee33ea48 |
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| Source note | uspto-grants-2000_03 |
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