反应详情

温度

70 °C

A mixture of 1-bromo-4-(7-bromoheptyloxy)benzene (4.405 g), cis-2,6-dimethylmorpholine (1.55 ml) and potassium carbonate (2.09 g) in N,N-dimethylformamide (22 ml) was stirred for 1 hour at 70° C. To the reaction mixture was added cis-2,6-dimethylmorpholine (7.75 ml) and stirred for 1 hour at 70° C. Ethyl acetate (100 ml) was added, and the mixture washed with water (50 ml×2) and brine. The separated organic layer was dried over magnesium sulfate and evaporated under reduced pressure to give a crude pale yellow oil (5.30 g). The crude oil was purified by silica gel chromatography (20:1-1:2 hexane-ethyl acetate) to give 4-[7-(4-bromophenoxy)heptyl]-cis-2,6-dimethylmorpholine (4.43 g) as a pale yellow oil.

1. stirringstirred for 1 hour at 70° C
2. washthe mixture washed with water (50 ml×2) and brine
3. dry with materialThe separated organic layer was dried over magnesium sulfate
4. customevaporated under reduced pressure
5. customto give a crude pale yellow oil (5.30 g)
6. customThe crude oil was purified by silica gel chromatography (20:1-1:2 hexane-ethyl acetate)