Hydrogen Peroxide → HCID 13134766, compound

HRID 482684Notes

Reaction equation

HRID 482684 reaction equation
OO.Cl.[CH3:4][C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:6]=1[NH:12][NH:13][C:14]1[S:15][CH2:16][CH2:17][N:18]=1.[OH-].[Na+]>C(Cl)Cl>[CH3:4][C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:6]=1[N:12]=[N:13][C:14]1[S:15][CH2:16][CH2:17][N:18]=1

Participants

5

Reactant 3

HCID 784Hydrogen Peroxide3×HCID 14798Sodium HydroxideHCID 13134759HCID 13134759, compound

Product 1

HCID 13134766HCID 13134766, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

3.5 ml of 30% strength perhydrol were added to a mixture of 6.5 g (0.025 mol) of 2-[2-(2,3-dimethylphenyl)-hydrazino]-2-thiazoline hydrochloride, 60 ml of methylene chloride and 50 ml of 2N sodium hydroxide solution. The mixture was stirred for 18 hours under reflux, and a further 2 ml of perhydrol were added after 6 hours, and another 1 ml of perhydrol after 12 hours. The organic phase was separated off, dried over potassium carbonate and evaporated down, and the residue was recrystallised from hexane/diethyl ether. Mp. 74° to 79°, yield 4.1 g (74% of theory).

Workup

  1. temperatureunder reflux
  2. customThe organic phase was separated off
  3. dry with materialdried over potassium carbonate
  4. customevaporated down
  5. customthe residue was recrystallised from hexane/diethyl ether

Sources & evidence

ORD record
ord-f8c2a018224849f9bbfb6a397fc53d32
Source dataset
uspto-grants-1986_03
Patent number
US04575501

Reaction notes

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