Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 67478765 | HCID 67478765 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 67478851 | HCID 67478851 | — |
Reaction Steps
To a suspension of (S)-N3-(5-cyclopropyl-1H-pyrazol-3-yl)-N1-[1-(4-fluorophenyl)ethyl]-4-nitrobenzene-1,3-diamine (Method 26; 0.37 g, 0.97 mmol) and Zinc dust (0.317 g, 4.85 mmol) in MeOH:THF (1:1, 24 ml) was slowly added saturated ammonium chloride (3.0 ml). The reaction mixture was stirred at 25° C. for 1 hr, to which was then added saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 min. Zn dust was removed by filtration and washed with EtOAc (20 ml). The organic layer was separated, washed with brine (10 ml), dried over Na2SO4, and concentrated. The crude product was used directly for the next step without further purification. MS: Calcd: 351; Found: [M+H]+ 352.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08129403B2 |
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| Source dataset | uspto-grants-2012_03 |
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| ORD ID | ord-c449fee717194a579a1c41f35d6dac54 |
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| Source note | uspto-grants-2012_03 |
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