Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 68521412 | HCID 68521412 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 68521596 | HCID 68521596 | — |
Reaction Steps
To a suspension of (S)-5-bromo-4-fluoro-N-(1-(4-fluorophenyl)ethyl)-2-nitrobenzenamine (Method 46; 0.63 g, 1.76 mmol) and zinc dust (0.554 g, 8.47 mmol) in MeOH:THF (1:1, 24 ml) was slowly added the saturated ammonium chloride solution (4 ml). The reaction mixture was stirred at 25° C. for 2 hours followed by addition of saturated ammonium acetate solution (5 ml). The resulting mixture was stirred for another 30 minutes. 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 under reduced pressure to give the crude product which was directly used for the next step without further purification. MS: Calcd.: 326. Found: [M+H]+ 327.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07622482B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-8d63911426e84c01a9a30fb4cfad3aab |
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| Source note | uspto-grants-2009_11 |
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