Potassium Iodide → HCID 67467398, compound
Reaction equation
[CH2:1]([CH:3]1[C:8]([C:9]2[CH:24]=[CH:23][C:12]3[N:13]=[C:14]([C:16]4[CH:21]=[CH:20][C:19]([OH:22])=[CH:18][CH:17]=4)[O:15][C:11]=3[CH:10]=2)=[N:7][NH:6][C:5](=[O:25])[CH2:4]1)[CH3:2].Cl[CH2:27][C:28](=[O:30])[CH3:29].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)=O>[CH2:1]([CH:3]1[C:8]([C:9]2[CH:24]=[CH:23][C:12]3[N:13]=[C:14]([C:16]4[CH:21]=[CH:20][C:19]([O:22][CH2:27][C:28](=[O:30])[CH3:29])=[CH:18][CH:17]=4)[O:15][C:11]=3[CH:10]=2)=[N:7][NH:6][C:5](=[O:25])[CH2:4]1)[CH3:2]Participants
6
Procedure
100 mg (298 μmol) 5-ethyl-6-[2-(4-hydroxy-phenyl)-benzoxazol-6-yl]-4,5-dihydro-2H-pyridazin-3-one, 24 μL (301 μmol) chloroacetone, 83 mg (601 μmol) potassium carbonate, 50 mg (301 μmol) potassium iodide and 10 ml acetone are heated together at 60° C. overnight. Then the mixture is extracted with 10% sodium carbonate solution and EA. The org. phase is washed with sat. saline solution, dried on sodium sulphate and then the solv. is totally eliminated i.V. The residue is purified through silica gel (eluant: DCM/methanol)
Workup
- extractionThen the mixture is extracted with 10% sodium carbonate solution and EA
- washphase is washed with sat. saline solution
- customdried on sodium sulphate
- customThe residue is purified through silica gel (eluant: DCM/methanol)
Sources & evidence
- ORD record
- ord-7c1623544f6e4bf6b0bc24a003d35f6c
- Source dataset
- uspto-grants-2014_07
- Patent number
- US08772323B2
Reaction notes
Loading…