3,5-Difluoro-2-hydrazinylpyridine → 3,5-Difluoropyridin-2-amine
Reaction equation
[NH:1]([C:3]1[C:8]([F:9])=[CH:7][C:6]([F:10])=[CH:5][N:4]=1)N>CO.[Ni]>[NH2:1][C:3]1[C:8]([F:9])=[CH:7][C:6]([F:10])=[CH:5][N:4]=1Participants
4
Reactant 1
Product 1
Reagents, catalysts & solvents 2
Procedure
Charged in a hydrogenation reactor were 500 ml of methanol, 14.5 g of the compound obtained in Step 4 and 11.5 g of Raney nickel as a catalyst, and H2 gas was introduced therein. The reactor was kept at room temperature for 24 hours, and the reaction mixture was filtered through Cellite® to remove the catalyst. The resulting solution was concentrated under a reduced pressure to obtain 10.8 g of the title compound as a light yellow solid (purity: 98.0%).
Workup
- additionCharged in a hydrogenation reactor
- additionH2 gas was introduced
- filtrationthe reaction mixture was filtered through Cellite®
- customto remove the catalyst
- concentrationThe resulting solution was concentrated under a reduced pressure
Sources & evidence
- ORD record
- ord-057a7ed5a273436abe021be72a2fd6d6
- Source dataset
- uspto-grants-2007_05
- Patent number
- US07220863B2
Reaction notes
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