反应详情

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).

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)