反应详情

To a solution of 10.1 ml of thionyl chloride in 50 ml of carbon tetrachloride was added, with stirring, a solution of 22.15 g of 1,4-bis(phenylmethyl)-2-piperazinemethanol in 120 ml of carbon tetrachloride. This mixture was stirred in an oil bath at 70° C. for one hour, then cooled in an ice bath and a solution of 17.1 9 of potassium hydroxide in 50 ml of water was added. The mixture was extracted several times with dichloromethane. The extracts were combined, filtered through hydrous magnesium silicate and evaporated. The residual gum was dissolved in warm heptane, filtered and evaporated to an oil which crystallized on standing, giving 17.94 g of 2-chloromethyl-1,4-bis(phenylmethyl)piperazine, mp 54°-56° oC.

1. stirringThis mixture was stirred in an oil bath at 70° C. for one hour
2. temperaturecooled in an ice bath
3. extractionThe mixture was extracted several times with dichloromethane
4. filtrationfiltered through hydrous magnesium silicate
5. customevaporated
6. dissolutionThe residual gum was dissolved in warm heptane
7. filtrationfiltered
8. customevaporated to an oil which
9. customcrystallized