反应详情

A mixture of 5.45 g. of 1-(2-naphthoylmethyl)imidazole hydrochloride, 2.49 g. ethylene glycol and 7.6 g. p-toluenesulfonic acid monohydrate in 50 ml. of toluene is heated overnight under reflux through a Dean-Stark trap. The trap is then replaced by a separatory funnel containing 4 A molecular seives and heating is continued for a further day. After cooling, the mixture is treated with 200 ml. of ethyl acetate, neutralized by pouring into excess aqueous potassium carbonate and the organic phase separated and dried (MgSO4) to afford a solution of 1-[2,2-ethylenedioxy-2-(2-naphthyl)ethyl]imidazole. The hydrochloride salt is prepared by dropwise addition of ethereal hydrogen chloride until precipitation is complete. Filtration and recrystallization from acetone/methanol gives 3.9 g. pure hydrochloride. m.p. 269°-270° C.

1. additionA mixture of 5.45 g
2. temperatureunder reflux through a Dean-Stark trap
3. customThe trap is then replaced by a separatory funnel
4. additioncontaining 4 A molecular seives
5. temperatureheating
6. waitis continued for a further day
7. temperatureAfter cooling
8. additionthe mixture is treated with 200 ml
9. customthe organic phase separated
10. dry with materialdried (MgSO4)