Hydrogen Peroxide → HCID 14098727, compound

HRID 1905377Notes

Reaction equation

HRID 1905377 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH2:12][CH:11]3[CH2:15][S:16](=[O:23])[C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1.[OH:24]O.O>C(O)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13](=[O:14])[CH2:12][CH:11]3[CH2:15][S:16](=[O:24])(=[O:23])[C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 14098716HCID 14098716, compound

Product 1

HCID 14098727HCID 14098727, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To a mixture of 4.7 g of 2-(4-chlorophenyl)-2,3,4,4a-tetrahydro-5H-(1)benzothiopyrano[4,3-c]pyridazin-3-one 6-oxide in 150 ml of acetic acid is added 55 ml of 35% hydrogen peroxide dropwise with stirring at room temperature. After the completion of addition, the mixture is stirred at 40°-50° C. on a water bath for 4 hours and poured into an excess amount of water. The precipitated crystals are collected by filtration and recrystallized from 50% aqueous solution of acetic acid to give 2.9 g of 2-(4-chlorophenyl)-2,3,4,4a-tetrahydro-5H-(1)benzothiopyrano[4,3-c]pyridazin-3-one 6,6-dioxide, melting at 168°-170° C., as a colorless powder.

Workup

  1. additionAfter the completion of addition
  2. stirringthe mixture is stirred at 40°-50° C. on a water bath for 4 hours
  3. filtrationThe precipitated crystals are collected by filtration
  4. customrecrystallized from 50% aqueous solution of acetic acid

Sources & evidence

ORD record
ord-f6cedb32ba734314905ec37a228e8054
Source dataset
uspto-grants-1989_06
Patent number
US04843075

Reaction notes

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