HCID 18919202, compound → HCID 18918911, compound
Reaction equation
[CH3:1][N:2]([CH3:14])[C:3]1[CH:8]=[N:7][N:6]([CH3:9])[C:5](=[O:10])[C:4]=1[CH:11]([OH:13])[CH3:12]>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[C:11]([C:4]1[C:5](=[O:10])[N:6]([CH3:9])[N:7]=[CH:8][C:3]=1[N:2]([CH3:14])[CH3:1])(=[O:13])[CH3:12]Participants
4
Reactant 1
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 50 °C
Procedure
In chloroform was dissolved 5-dimethylamino-4-(1-hydroxy)ethyl-2-methyl-3(2H)-pyridazinone (355 mg) followed by addition of active manganese dioxide (2.0 g), and the mixture was stirred at 50° C. for 24 hours. After the oxidizing agent was filtered off, the filtrate was concentrated and the residue was washed with n-hexane and diethyl ether and dried. Yellow powder, 178 mg. 1 H-NMR (CDCl3) E: 2.6.7(3H,s), 2.94(6H,s), 3.69(3H,s), 7.66(1H,s).
Workup
- filtrationAfter the oxidizing agent was filtered off
- concentrationthe filtrate was concentrated
- washthe residue was washed with n-hexane and diethyl ether
- customdried
Sources & evidence
- ORD record
- ord-f3c0ab55b6d24549b394d3a1a6620044
- Source dataset
- uspto-grants-1998_05
- Patent number
- US05753664
Reaction notes
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