反应详情

To a solution of 3.02 g of (E)-1-cinnamyl-3-(3-pyridyl)imidazolidine-2-thione dissolved in 40 ml of 4N hydrochloric acid, 10 ml of an aqueous solution of 1.03 g of NaNO2 was added dropwise. After stirring at room temperature for 1 hour, the mixture was made alkaline by addition of a sodium hydroxide solution, and the precipitated crystals were collected by filtration. The crystals obtained were washed with water, dried and then purified by silica gel column chromatorgraphy (solvent: chloroform-methanol=30:1), followed by recrystallization from ethanol, to give 1.74 g of (E)-1-cinnamyl-3-(3-pyridyl)-2-imidazolidinone.

1. filtrationthe precipitated crystals were collected by filtration
2. customThe crystals obtained
3. washwere washed with water
4. customdried
5. custompurified by silica gel column chromatorgraphy (solvent: chloroform-methanol=30:1)
6. customfollowed by recrystallization from ethanol