Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 10570553 | HCID 10570553 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Product | HCID 10643284 | HCID 10643284 | — |
Reaction Steps
To a solution of 1.0 g of 2-(4-chlorophenyl)-9-methyl-5,6-dihydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one in 50 ml of formic acid is added 0.3 ml of 35% aqueous hydrogen peroxide solution with stirring at 5° C. and the mixture is stirred for 10 minutes at the same temperature. To the mixture is further added 0.3 ml of aqueous hydrogen peroxide solution and the mixture is stirred for 20 minutes. Then, the mixture is poured into water, extracted with chloroform three times and the extract is washed with water and dried over magnesium sulfate. After the chloroform is distilled off under reduced pressure, the resulting crystals are recrystallized from a mixed solvent of chloroform and ethanol to give 1.0 g of 2-(4-chlorophenyl)-9-methyl-5,6-dihydrothieno[2',3':2,3]thiepino[4,5-c]pyridazin-3(2H)-one 7-oxide as white crystals, melting at 174°-175° C. with decomposition.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05329016 |
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| Source dataset | uspto-grants-1994_07 |
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| ORD ID | ord-d78a80da2ea646ba833b45fd8a153087 |
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| Source note | uspto-grants-1994_07 |
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