反应详情

温度

140 °C

8.7 g of 2,2-dimethyl-5-trifluoromethylsulfonyloxy-4H-(1,3)benzodioxin-4-one, 23.2 g of 2-methoxy-5-tributylstannylpyridine, 3.4 g of lithium chloride, 0.6 g of tetrakistriphenylphosphinepalladium0 and 70 mg of 2,6-di-t-butyl-4-methylphenol are dissolved in 150 ml of dioxane and the mixture is stirred for 3 h at 140° C. in an autoclave. It is then concentrated under reduced pressure, the residue is stirred with 200 ml of n-pentane and filtered on a little silica gel 60, the latter is subsequently washed with n-pentane and the product is eluted using ethyl acetate. After concentration, 10.3 g of m.p. 160° C. remain.

1. concentrationIt is then concentrated under reduced pressure
2. stirringthe residue is stirred with 200 ml of n-pentane
3. filtrationfiltered on a little silica gel 60
4. washthe latter is subsequently washed with n-pentane
5. washthe product is eluted
6. concentrationAfter concentration, 10.3 g of m.p. 160° C.