Nitric Acid → 5-Bromo-6-methyl-3-nitropyridine-2-amine
Reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([Br:9])=[CH:4][CH:3]=1.[N+:10]([O-])([OH:12])=[O:11].[OH-].[Na+]>S(=O)(=O)(O)O>[Br:9][C:5]1[C:6]([CH3:8])=[N:7][C:2]([NH2:1])=[C:3]([N+:10]([O-:12])=[O:11])[CH:4]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
20 g(0.107 mole) of the compound obtained in step 1 was dissolved in 110 ml of conc. sulfuric acid and thereto was added dropwise 9.4 ml(0.12 mole) of nitric acid for 30 minutes at 0° C. The reaction solution was stirred for 1 hour at 0° C. and, subsequently stirred for another 1 hour at room temperature. The resultant was neutralized with cold 40% aqueous NaOH solution and filtered to get a yellow solid. The solid was washed with distilled water(100 ml×3) and dried in a vacuum oven at 60° C. for 24 hours to obtain 23.8 g of the title compound(yield 96%).
Workup
- stirringsubsequently stirred for another 1 hour at room temperature
- filtrationfiltered
- customto get a yellow solid
- washThe solid was washed with distilled water(100 ml×3)
- customdried in a vacuum oven at 60° C. for 24 hours
Sources & evidence
- ORD record
- ord-3b96db20fb72461ebd5aeb7efce2b21c
- Source dataset
- uspto-grants-1998_12
- Patent number
- US05849753
Reaction notes
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