反应详情

A suspension of 9.84 g of 2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine, 1.4 g of tetra-n-butylammonium sulfate and 7.56 g of 2-chloromethyl-pyridine N-oxide hydrochloride in 140 ml of toluene is treated with 30 ml of 28 percent sodium hydroxide while stirring vigorously. The temperature rises immediately to 30°. After 2 hours, the precipitate is removed by filtration under suction, washed with water and dried at 60° in vacuo. From methanol and acetonitrile there is obtained 2-([{2-[(2,6-dichlorophenyl)imino]-1-imidazol idinyl}oxy]methyl)-pyridine 1-oxide of melting point 185°-187°. The corresponding hydrochloride crystallizes from methanol/acetonitrile with 2.5 mol of hydrochloric acid and melts at 171°-173°. The corresponding cyclohexylsulfamate decomposes slowly from 159°-238°.

1. customrises immediately to 30°
2. customthe precipitate is removed by filtration under suction
3. washwashed with water
4. customdried at 60° in vacuo