反应详情

温度

33 °C

15 grams of 1-(2-diethylaminoethyl)-2-hydroxy-6-chloro-7-aza-benzimidazole were dissolved in 200 ml of concentrated hydrochloric acid and there were added in portions with stirring 24.5 grams of potassium chlorate at room temperature. The temperature increased temporarily to 33° C. The mixture was stirred for another hour, made alkaline with sodium hydroxide, the mixture extracted with shaking with n-butanol, the extract evaporated in a vacuum and the residue chromatographed over silica gel. The reaction product was recrystallized from ethyl acetate. M.P. 137°-139° C.; Yield: 3 grams.

1. additionthere were added in portions
2. extractionthe mixture extracted
3. stirringwith shaking with n-butanol
4. customthe extract evaporated in a vacuum
5. customthe residue chromatographed over silica gel
6. customThe reaction product was recrystallized from ethyl acetate