2,2-Diethoxyethylamine → HCID 178422435, compound

HRID 1736401Notes

Reaction equation

HRID 1736401 reaction equation
C(O[CH:4](OCC)[CH2:5][NH2:6])C.[Br:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]=[C:18]=[S:19])=[C:13]([CH3:20])[CH:12]=1>Cl>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]2[CH:4]=[CH:5][N:6]=[C:18]2[SH:19])=[C:13]([CH3:20])[CH:12]=1

Participants

4

Reactant 2

HCID 695242,2-DiethoxyethylamineHCID 879774-Bromo-1-isothiocyanato-2-methylbenzene

Product 1

HCID 178422435HCID 178422435, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

105.5 Milliliters of 2,2-diethoxyethylamine was dropwise added to 138 g of 4-bromo-2-methylphenyl isothiocyanate with ice-cooling. The mixture was stirred for 10 minutes and then further stirred for 10 minutes at 100° C. The mixture was allowed to cool, and thereto was added 500 ml of 8 N hydrochloric acid. The mixture was refluxed for 2 hours. The resulting crystals were collected by filtration, washed with water thoroughly and then dried to obtain 110 g of 1-(4-bromo-2-methylphenyl)-2-mercaptoimidazole.

Workup

  1. temperaturecooling
  2. stirringfurther stirred for 10 minutes at 100° C
  3. temperatureto cool
  4. temperatureThe mixture was refluxed for 2 hours
  5. filtrationThe resulting crystals were collected by filtration
  6. washwashed with water thoroughly
  7. customdried

Sources & evidence

ORD record
ord-2b01daf0d3ed418bb910c42e792e2650
Source dataset
uspto-grants-1996_07
Patent number
US05541198

Reaction notes

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