O-Xylene → HCID 67078397, compound
Reaction equation
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([Br:9])=[CH:4][N:3]=1.C[CH2:11][O:12]C(C1C(=O)CCCC1)=O.[C:22]1(C)[C:23](C)=[CH:24][CH:25]=[CH:26][CH:27]=1>>[Br:9][C:5]1[CH:6]=[C:7]2[NH:8][C:11](=[O:12])[N:1]([C:27]3[CH2:26][CH2:25][CH2:24][CH2:23][CH:22]=3)[C:2]2=[N:3][CH:4]=1Participants
4
Procedure
2,3-Diamino-5-bromopyridine (50 g) and 2-cyclohexanonecarboxylic acid ethyl ester (63.5 ml) were heated under reflux in xylene (2000 ml) for 64 hours. The reaction solution was cooled to room temperature and the precipitated crystals were collected by filtration. The resulting crude crystals were recrystallized from toluene to give the title compound (30 g).
Workup
- filtrationthe precipitated crystals were collected by filtration
- customThe resulting crude crystals were recrystallized from toluene
Sources & evidence
- ORD record
- ord-ab878942854a464fa73ff5998127cd52
- Source dataset
- uspto-grants-2014_07
- Patent number
- US08785438B2
Reaction notes
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