Hydrochloric Acid → HCID 178432906, compound

HRID 1580106Notes

Reaction equation

HRID 1580106 reaction equation
[NH:1]1[CH:5]=[C:4]([S:6]([N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[CH3:14])(=[O:8])=[O:7])[N:3]=[CH:2]1.[ClH:15]>C(O)C>[ClH:15].[NH:1]1[CH:5]=[C:4]([S:6]([N:9]2[CH:13]=[CH:12][N:11]=[C:10]2[CH3:14])(=[O:7])=[O:8])[N:3]=[CH:2]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 1784329051-(4-Imidazolylsulfonyl)-2-methylimidazole

Product 1

HCID 178432906HCID 178432906, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of 2.12 g of 1-(4-imidazolesulfonyl)-2-methylimidazole from Example 2 was dissolved in 100 ml of absolute ethanol in a dry flask equipped with a drying tube. A 50 ml aliquot of saturated ethereal hydrogen chloride was added over a five minute period. No precipitate formed immediately but did after about 15 minutes. The mixture was chilled in an ice bath for an additional 30 minutes and the precipitate filtered under a nitrogen atmosphere and dried under vacuum. The yield of white crystals of the hydrochloride of 1-(4-imidazolylsulfonyl)-2-methylimidazole was 1.87 g with mp 195°-8°. An analytical sample was made by recrystallization from ethanol and ether mixture, λmaxnujol 3.15-4.1 (NR3 +Cl-), 7.20 (SO2N) and 8.52 μ (SO2N).

Workup

  1. customequipped with a drying tube
  2. customNo precipitate formed immediately
  3. temperatureThe mixture was chilled in an ice bath for an additional 30 minutes
  4. filtrationthe precipitate filtered under a nitrogen atmosphere
  5. customdried under vacuum
  6. customAn analytical sample was made by recrystallization from ethanol and ether mixture, λmaxnujol 3.15-4.1 (NR3 +Cl-), 7.20 (SO2N) and 8.52 μ (SO2N)

Sources & evidence

ORD record
ord-13ab5a53d410486390f386bc21e6b1d0
Source dataset
uspto-grants-1976_01
Patent number
US03932444

Reaction notes

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