Hydrochloric Acid → HCID 23446966, compound
Reaction equation
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([CH3:11])([CH3:10])[CH3:9])[C:3]=1[N+:12]([O-])=O.[ClH:15].O>C(O)C.[Pd]>[ClH:15].[ClH:15].[NH2:12][C:3]1[C:4]([C:8]([CH3:11])([CH3:10])[CH3:9])=[N:5][N:6]([CH3:7])[C:2]=1[NH2:1]Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
A suspension of 8.5 g (0.035 mol) of 5-amino-1-methyl-4-nitro-3-tert-butylpyrazole and 1.5 g of 5% by weight palladium-on-charcoal containing 50% water in 200 cm3 of ethanol was placed in a hydrogenator. After stirring for 3 hours under a hydrogen pressure of 10 bar, at a temperature of 75° C., the reaction medium was poured into a solution, precooled to 0° C., of 60 cm3 of ethanol and 20 cm3 of 12N hydrochloric acid. The solution was clarified by filtration on a sinter funnel and then evaporated to dryness under reduced pressure. The brown solid obtained was taken up, at reflux, in 35 cm3 of 5N hydrochloric ethanol and 11 cm3 of water and then cooled to room temperature. The white crystals obtained were filtered off on a sinter funnel and then dried under vacuum at room temperature. 4.9 g of the expected product were obtained in the form of white crystals, the melting point of which was 260° C. The elemental analysis for C8H10N4.2HCl was:
Workup
- additionat a temperature of 75° C., the reaction medium was poured into a solution
- filtrationThe solution was clarified by filtration on a sinter funnel
- customevaporated to dryness under reduced pressure
- customThe brown solid obtained
- customThe white crystals obtained
- filtrationwere filtered off on a sinter funnel
- customdried under vacuum at room temperature
Sources & evidence
- ORD record
- ord-90944420aeca408aa2df151ee7274377
- Source dataset
- uspto-grants-2000_08
- Patent number
- US06099592
Reaction notes
Loading…