Hydrogen Peroxide → HCID 501201, compound

HRID 2300991Notes

Reaction equation

HRID 2300991 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH2:9][S:10][C:11]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][N+:12]=1[O-:18].OO.[OH:21]S([O-])=O.[Na+]>CO.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[CH2:9][S:10]([C:11]1[C:16]([CH3:17])=[CH:15][CH:14]=[CH:13][N+:12]=1[O-:18])=[O:21]

Participants

6

Reactant 3

HCID 784Hydrogen PeroxideHCID 501202HCID 501202, compoundHCID 23665763Sodium Bisulfite

Product 1

HCID 501201HCID 501201, compound

Reagents, catalysts & solvents 2

HCID 26052Sodium tungstateCatalystHCID 887MethanolSolvent

Conditions

Temperature
25 °C

Procedure

To 10.5 g (0.035 mole) of 2-[(2,6-dichlorophenyl)methylthio]-3-methyl-pyridine-N-oxide (See Example 28 above) dissolved in 100 ml of methanol were added a pinch of sodium tungstate and then dropwise 4.2 ml (0.4 mole) of 50% hydrogen peroxide. The temperature was maintained at 25° C. for four hours, and then a cold solution of NaHSO3 was added slowly to destroy residual H2O2. The solid was filtered and air-dried, having a melting point of 178-181° C., yield 10 g. The elemental analysis for C,H,N; the infrared spectrum, and the NMR spectrum all supported the proposed structure.

Workup

  1. customto destroy residual H2O2
  2. filtrationThe solid was filtered
  3. customair-dried

Sources & evidence

ORD record
ord-5f4646f6a5614b7eacb279d4bbd83beb
Source dataset
uspto-grants-2002_12
Patent number
US06498254B1

Reaction notes

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