HCID 131735472, compound → HCID 76847321, compound
Reaction equation
[Cl:1][C:2]1[C:3]([CH:13]=[CH:14][N:15](C)C)=[C:4]([N+]([O-])=O)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[H][H]>C(OCC)(=O)C.[Ni]>[Cl:1][C:2]1[CH:7]=[N:6][C:5]([O:8][CH3:9])=[C:4]2[NH:15][CH:14]=[CH:13][C:3]=12Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
To a solution of Example 108C (12 g, 46.6 mmol) in ethyl acetate (150 mL) was added Raney-Ni (20.0 g, 4.66 mmol), and the reaction mixture was stirred for 20 hours at room temperature under 30 atm. hydrogen. The reaction mixture was filtered and rinsed with ethyl acetate. The filtrate was concentrated to a small volume, and the precipitates were collected by filtration and dried to provide the title compound (10 g, 93% yield).
Workup
- filtrationThe reaction mixture was filtered
- washrinsed with ethyl acetate
- concentrationThe filtrate was concentrated to a small volume
- filtrationthe precipitates were collected by filtration
- customdried
Sources & evidence
- ORD record
- ord-dcae7173ec4c4e5c95afe1a6aa561342
- Source dataset
- uspto-grants-2016_04
- Patent number
- US09321764B2
Reaction notes
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