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To a solution of 34.5g Mg turnings in 215mL dried Et2O was dropwise added a solution of 225g(a) in 500mL dried Et2O at reflux temperature. After continuing to 30min. stirring at reflux, then the resulting Grignard solution was added under stirring and room temperature into a solution of 218a in 712mL dried Et2O. The mixture was stirred for another 4 hrs at 25oC, then 100mL glacial HOAc was added, the resulting mixture was poured into water. The organic phase was separated, the aq. phase was extracted with Et2O, the combining org. phase was washed with NaHCO3 solution and water successively, dried over Na2SO4 and removal of solvent in vacuo gave the white 358.6g (b).
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Originally posted by zhonghu at 2008-4-22 18:00:
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