Potassium Hydroxide → HCID 21449315, compound

HRID 596946Notes

Reaction equation

HRID 596946 reaction equation
Cl[O-].[Na+].[OH-].[K+].[NH2:6][C:7]1[CH:12]=[C:11]([S:13][C:14]2[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=2)[CH:10]=[CH:9][C:8]=1[N+:21]([O-:23])=[O:22]>C(O)C>[CH3:20][C:17]1[CH:16]=[CH:15][C:14]([S:13][C:11]2[CH:10]=[CH:9][C:8]3[C:7]([CH:12]=2)=[N:6][O:22][N+:21]=3[O-:23])=[CH:19][CH:18]=1

Participants

5

Reactant 3

HCID 14797Potassium HydroxideHCID 203628195-[(4-Methylphenyl)sulfanyl]-2-nitroanilineHCID 23665760Sodium Hypochlorite

Product 1

HCID 21449315HCID 21449315, compoundYield 83.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

60 ml of sodium hypochlorite solution (13%) is added dropwise at ca. 30° C internal temperature, with continuous stirring, to a solution of 3 g of potassium hydroxide in 150 ml of ethanol and 7 g of 2-amino-4-(4'-methylphenylthio)-nitrobenzene. After completion of the addition, stirring is continued for half an hour at room temperature; the precipitated product is filtered off with suction and then washed with 200 ml of water. Recrystallisation from ethanol yields 5.8 g (= 83.5% of theory) of 5-(4'-methylphenylthio)-benzofurazan-N-oxide, M.P. 86°-88° C.

Workup

  1. additionAfter completion of the addition
  2. waitis continued for half an hour at room temperature
  3. filtrationthe precipitated product is filtered off with suction
  4. washwashed with 200 ml of water
  5. customRecrystallisation from ethanol

Sources & evidence

ORD record
ord-7b8a9d91af3745d1a4f6a32fa5fef4e4
Source dataset
uspto-grants-1977_03
Patent number
US04012512

Reaction notes

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