n-Methyl-3-nitropyridin-4-amine → 4-N-methylpyridine-3,4-diamine
Reaction equation
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[N+:9]([O-])=O.[H][H]>CO.[Ni]>[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[NH2:9]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
2.3 g methyl-(3-nitropyridin-4-yl)-amine are hydrogenated in 50 ml of methanol for and with 0.8 g Raney nickel for 2.5 h at 50° C. and 50 psi hydrogen pressure. The catalyst is filtered off and the filtrate is evaporated to dryness. The product is purified by chromatography (Alox, dichloromethane/methanol from 99/1 to 19/1). 1.55 g product are obtained as a solid.
Workup
- customfor 2.5 h
- customat 50° C.
- filtrationThe catalyst is filtered off
- customthe filtrate is evaporated to dryness
- customThe product is purified by chromatography (Alox, dichloromethane/methanol from 99/1 to 19/1)
Sources & evidence
- ORD record
- ord-15a1784810ef4e29b7c08e8f34ae74ca
- Source dataset
- uspto-grants-2014_06
- Patent number
- US08754073B2
Reaction notes
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