5-Bromopyridine-2,3-diamine → HCID 178422994, compound
Reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[N:6][CH:7]=1.[CH3:10][C:11]1[CH:16]=[C:15]([C:17](O)=O)[CH:14]=[CH:13][N:12]=1>O>[Br:1][C:2]1[CH:3]=[C:4]2[N:9]=[C:17]([C:15]3[CH:14]=[CH:13][N:12]=[C:11]([CH3:10])[CH:16]=3)[NH:8][C:5]2=[N:6][CH:7]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
0.30 g 5-bromo-2,3-diaminopyridine and 0.212 g 2-methyl-pyridine-4-carboxylic acid were heated in 3 g polyphosphoric acid at 160° C. with stirring for 16 hrs. The mixture was diluted with water and insoluble components removed by filtration. Water was evaporated from the filtrate and the residue dispersed in pyridine. Again, insoluble components were removed by filtration and the filtrate evaporated. The obtained residue was washed thoroughly with water and dried.
Workup
- customremoved by filtration
- customWater was evaporated from the filtrate
- additionthe residue dispersed in pyridine
- customAgain, insoluble components were removed by filtration
- customthe filtrate evaporated
- washThe obtained residue was washed thoroughly with water
- customdried
Sources & evidence
- ORD record
- ord-9e7640a98ba34f91a1743d42bec42562
- Source dataset
- uspto-grants-2009_11
- Patent number
- US07618964B2
Reaction notes
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