Hydrochloric Acid → HCID 178481665, compound

HRID 1862800

Reaction equation

HRID 1862800 reaction equation
Cl.[CH3:2][NH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH2:10].[C:11](=[S:13])=S.[OH-].[Na+].Cl>C(O)C.O>[SH:13][C:11]1[N:3]([CH3:2])[C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[N:10]=1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 6348Carbon DisulfideHCID 14798Sodium HydroxideHCID 17372766N~1~-Methylbenzene-1,2-diamine--hydrogen chloride (1/1)

Product 1

HCID 178481665HCID 178481665, compoundYield 67%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

11.7 g of N-methyl-o-phenylenediamine hydrochloride, 9.1 g of carbon disulfide and an aqueous solution containing 7.2 g of sodium hydroxide and 20 ml of water were added to 150 ml of ethanol and the mixture was heated and refluxed for 4 hours. After cooling, a 3 N hydrochloric acid aqueous solution was added to the reaction mixture to make the reaction solution slightly acidic and, thereby, crystals were precipitated. After filtration, the crystals were recrystallized from a mixture of water and ethanol (70:30 by volume) to obtain 6 g of 2-mercapto-1-methylbenzimidazole (Compound (III-11)) having a melting point of 194° to 195° C. (yield: 67%).

Workup

  1. temperaturethe mixture was heated
  2. temperaturerefluxed for 4 hours
  3. temperatureAfter cooling
  4. customcrystals were precipitated
  5. filtrationAfter filtration
  6. customthe crystals were recrystallized from a mixture of water and ethanol (70:30 by volume)

Sources & evidence

ORD record
ord-b1428663e16a4ab593f2fbf436cf595f
Source dataset
uspto-grants-1979_09
Patent number
US04166742

Linked notes

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