HCID 21479602, compound → HCID 21479615, compound

HRID 2292966Notes

Reaction equation

HRID 2292966 reaction equation
[I:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[CH2:16][CH2:15][CH2:14][C:13]([C:17]3[CH:22]=[CH:21][C:20]([S:23][CH3:24])=[CH:19][CH:18]=3)=[N:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.I([O-])(=O)(=O)=[O:26].[Na+]>CO.O>[I:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[CH2:16][CH2:15][CH2:14][C:13]([C:17]3[CH:18]=[CH:19][C:20]([S:23]([CH3:24])=[O:26])=[CH:21][CH:22]=3)=[N:12]2)(=[O:9])=[O:10])=[CH:4][CH:3]=1

Participants

5

Reactant 2

HCID 21479602HCID 21479602, compoundHCID 23667635Sodium periodate

Product 1

HCID 21479615HCID 21479615, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

A solution of 1-(4Iodobenzenesulfonyl)-3-(4-methylthiophenyl)-1,4,5,6-tetrahydropyridazine (1.27 g, 2.69 mmol) in methanol (450 mL) was added to a solution of sodium periodate (0.61 g, 2.82 mmol) in water (6 mL) and stirred at a low heat for 16 hours. The resulting mixture was filtered, concentrated arylphosphonyl dihalide and purified by column chromatography on silica gel using ether/methylene chloride as an eluent to give the title compound as a solid: mp 191°-193° C.

Workup

  1. temperaturea low heat for 16 hours
  2. filtrationThe resulting mixture was filtered
  3. customconcentrated arylphosphonyl dihalide and purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-5aa711cd7fee4cf089d2d88e4d250fe3
Source dataset
uspto-grants-1997_11
Patent number
US05684151

Reaction notes

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