Hydrogen Peroxide → HCID 14578923, compound

HRID 231783Notes

Reaction equation

HRID 231783 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](=[O:24])[C:18]4[CH:23]=[CH:22][CH:21]=[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])(=[O:24])[C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=4[C:10]3=[N:9]2)=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 784Hydrogen PeroxideHCID 962WaterHCID 1952532-(4-Chlorophenyl)-5,6-dihydro-(1)-benzothiepino(5,4-c)pyridazin-3(2H)-one-7-oxide

Product 1

HCID 14578923HCID 14578923, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

To a solution of 14 g of 2-(4-chlorophenyl)-5,6-dihydro-[1]benzothiepino[5,4-c]pyridazin-3(2H)-one 7-oxide prepared in Example 14 in 200 ml of acetic acid is added 15 ml of hydrogen peroxide with stirring at room temperature. The mixture is stirred at 50°-55° C. for 2 hours, poured into 1 liter of water and the precipitated crystals are collected by filtration. The crude products obtained are purified by column chromatography on silica gel and recrystallized from chloroform-methanol to give 9.8 g of 2-(4-chlorophenyl-5,6-dihydro-[1]benzothiepino[5,4-c]pyridazin-3(2H)-one 7,7-dioxide, melting at above 310° C.

Workup

  1. stirringThe mixture is stirred at 50°-55° C. for 2 hours
  2. filtrationthe precipitated crystals are collected by filtration
  3. customThe crude products obtained
  4. customare purified by column chromatography on silica gel
  5. customrecrystallized from chloroform-methanol

Sources & evidence

ORD record
ord-82ad3972bae44a1dbb7529df77ed5a5d
Source dataset
uspto-grants-1989_07
Patent number
US04849421

Reaction notes

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