HCID 18704056, compound → HCID 18704058, compound
Reaction equation
[CH3:1][C:2]1[C:11]([N+:12]([O-])=O)=[CH:10][C:5]2=[N:6][C:7](=[O:9])[N:8]=[C:4]2[CH:3]=1.[H][H]>N.O[V](=O)=O.[O-2].[O-2].[Ti+4].[Pd].O>[NH2:12][C:11]1[C:2]([CH3:1])=[CH:3][C:4]2=[N:8][C:7](=[O:9])[N:6]=[C:5]2[CH:10]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 4
Conditions
- Temperature
- 65 °C
Procedure
0.01 g of ammonium vanadate and 5 g of titanium dioxide extrudate containing 1% by weight of metallic palladium and having a particle size of 3 mm (from Johnson Matthey) are added to a suspension consisting of 500 ml of water and 19.3 g of 5-methyl-6-nitrobenzimidazolone. After displacing the air with nitrogen, the latter is replaced by hydrogen at atmospheric pressure and the suspension is stirred at 65° C. for 78 hours. During this time, 105% of the theoretical amount of hydrogen, based on the 5-methyl-6-nitrobenzimidazolone, is adsorbed. The resulting suspension is then sieved through a sieve having a mesh width of 1 mm. The material remaining on the sieve is washed with 100 ml of water and the combined aqueous phases are then filtered through a paper filter and washed with 50 ml of water. Drying at 80° C. under reduced pressure (125 mbar) gives 15.1 g (93%) of 5-amino-6-methylbenzimidazolone.
Workup
- additionare added to a suspension
- filtrationThe resulting suspension is then sieved through a sieve
- washis washed with 100 ml of water
- filtrationthe combined aqueous phases are then filtered through a paper
- filtrationfilter
- washwashed with 50 ml of water
- customDrying at 80° C. under reduced pressure (125 mbar)
Sources & evidence
- ORD record
- ord-c827a5ec29c14180978f82b46db8ae8c
- Source dataset
- uspto-grants-2000_07
- Patent number
- US06087480
Reaction notes
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