反应详情

温度

80 °C

The 4-phenyl-1,3,2-dioxaborolane was first prepared by reaction of 236 mg phenyl-1,2-ethanediol (1.7 mmol) with borane dimethylsulfide adduct (0.15 ml, 1.5 mmol) in 2 ml of dioxane. A stock solution of the catalyst in dioxane was made by heating 250 mg PdCl2[dppf].CH2Cl2 with triethylamine (4.5 ml) at 80° C. for 20 h in 40 ml dioxane. To this solution was added 2.48 g (10 mmol) of 1-iodo-3,4-methylenedioxybenzene. 4.8 ml of this reaction solution was then placed in the reaction tube containing the borane ester. The mixture was heated for 20 h at 80° C. and then an aliquot was removed, dissolved in some ethyl acetate containing a little of the diol and shaken with 10% brine solution. After drying with MgSO4, the gc was measured. One major peak, of retention time 15.7 mins was found. This was shown by gc/ms to be the desired product.

1. customan aliquot was removed
2. dissolutiondissolved in some ethyl acetate containing a little of the diol
3. dry with materialAfter drying with MgSO4