Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 11502190 | HCID 11502190 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 67478890 | HCID 67478890 | — |
Reaction Steps
To a suspension of (S)-N1-(5-cyclopropyl-1H-pyrazol-3-yl)-4-fluoro-N3-[1-(4-fluorophenyl)ethyl]-6-nitrobenzene-1,3-diamine (Method 38; 0.33 g, 0.826 mmol) and Zinc dust (0.270 g, 4.13 mmol) in MeOH:THF (1:1, 10 ml) was slowly added saturated ammonium chloride (4 ml). The mixture was stirred at 25° C. for 2 hrs, to which was added saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 min. The Zn dust was removed by filtration and washed with EtOAc (15 ml). The organic layer was separated and dried over Na2SO4. After removal of solvent, the title compound was used directly for the next step without further purification.
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-ad605449eab24bc9af7909745d476169 |
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| Source note | uspto-grants-2012_03 |
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