Hydrogen Peroxide → HCID 14578915, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH:12]=[C:11]3[CH2:15][CH2:16][S:17][C:18]4[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1.[OH:25]O.O>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH:12]=[C:11]3[CH2:15][CH2:16][S:17](=[O:25])[C:18]4[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 1.8 g of 2-(4-chlorophenyl)-10-fluoro-5,6-dihydro-[1]benzothiepino[5,4-c]pyridazin-3(2H)one, prepared in Example 22, in 20 ml of acetic acid is added 1.3 ml of 35% hydrogen peroxide with stirring at room temperature and furthermore stirred for 5 hours at the same temperature. To the resultant mixture is added water, and the precipitated crystals are collected by filtration and recrystallized from dimethylformamide-water to give 1.3 g of 2-(4-chlorophenyl)-10-fluoro-5,6-dihydro[1]benzothiepino[5,4-c]pyridazin-3(2H)-one 7-oxide, melting at 233°-235° C. with decomposition.
Workup
- stirringfurthermore stirred for 5 hours at the same temperature
- filtrationthe precipitated crystals are collected by filtration
- customrecrystallized from dimethylformamide-water
Sources & evidence
- ORD record
- ord-dd65fd2946a34080a58d55a4a10b0151
- Source dataset
- uspto-grants-1989_07
- Patent number
- US04849421
Reaction notes
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