Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 459019 | HCID 459019 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | HCID 458932 | HCID 458932 | 86.6% |
Reaction Steps
A mixture of zinc powder (2 g) and ammonium chloride (0.2 g) in 22 ml of a water/ethanol mixture (1/1) was refluxed in a boiling-water bath. The derivative N-{2-[(4nitrophenyl)amino]ethyl}benzenesulfonamide (2) (3 g, 9 mmol) was added in portions and heating was continued until the reaction medium decolorized. The mixture was filtered while hot and the zinc was rinsed with ethanol/water solution (50/50). The filtrate crystallized rapidly. After cooling to 0° C., the solid was filtered off and then washed with water. After drying, 2.27 g of crude product with a melting point of 144° C. were obtained. 0.77 g of this crude product was recrystallized from 20 mL of water/ethanol (1/1), and the crystals obtained were dried over P2O5 and microanalysed.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07347879B2 |
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| Source dataset | uspto-grants-2008_03 |
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| ORD ID | ord-913d8433d0c04c6db0e727bf7c61052d |
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| Source note | uspto-grants-2008_03 |
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