反应详情

A solution of methyl 4-(4-biphenylylmethoxy)phenylacetate (60.0 g), N,N-dimethylethylenediamine (47.7 g), and 1H-1,2,4-triazole (12.6 g) in toluene (120 ml) was stirred under nitrogen at 100° C. for 8 hr and cooled until the temperature of the reaction mixture was reached to 60±2° C., to which ethyl acetate (240 ml) was added for 20 min. The reaction mixture was further heated under reflux for additional 30 min, left to stand at room temperature over night and stirred in an ice bath for 2 hr. The precipitate was collected by filtration and washed with ethyl acetate (120 ml) to obtain the titled compound (71.7 g).

1. temperaturecooled until the temperature of the reaction mixture
2. additionwas added for 20 min
3. temperatureThe reaction mixture was further heated
4. temperatureunder reflux for additional 30 min
5. waitleft
6. waitto stand at room temperature over night
7. filtrationThe precipitate was collected by filtration
8. washwashed with ethyl acetate (120 ml)