反应详情

A suspension of phenylboronic acid (0.5 g, 4.1 mmol), copper(II)-acetate-1-hydrate (0.041 g, 0.21 mmol) and molecular sieves (1.5 g, size 0.4 nm, powdered) in dichloromethane (12 ml) was stirred for 5 min. Then 2-(aminomethyl)-1,3-dioxolane (0.211 g, 2.05 mmol) was added and oxygen was bubbled through the mixture for 5 min. The vessel was closed and shaken overnight at room temperature. For workup ethyl acetate (50 ml) and 1 M sodium bicarbonate solution (30 ml) were added and the mixture was shaken. The organic layer was separated, dried over magnesium sulfate and evaporated. The residue was purified using flash chromatography (SiO2; eluent: heptane/ethyl acetate=90:10) to yield a light yellow oil (105 mg, 14%); MS (EI): 179.1 (M+.).

1. customoxygen was bubbled through the mixture for 5 min
2. customThe vessel was closed
3. stirringshaken overnight at room temperature
4. additionFor workup ethyl acetate (50 ml) and 1 M sodium bicarbonate solution (30 ml) were added
5. stirringthe mixture was shaken
6. customThe organic layer was separated
7. dry with materialdried over magnesium sulfate
8. customevaporated
9. customThe residue was purified