反应详情

9.5 g (27.9 mmol) of 2-iodo-9,10-dihydrophenanthrene are dissolved in 40 ml of trimethyl phosphate, and a solution of 2 ml (39 mmol) of bromine in 10 ml of trimethyl phosphate is added dropwise at 20° C. After 90 min, the batch is added to ice-water, excess bromine is reduced by addition of sodium hydrogensulfite soln., and the precipitated product is filtered off with suction, taken up in toluene, washed with sat. sodium hydrogen-carbonate soln. and dried over sodium sulfate. The solvent is removed in vacuo, and the residue is recrystallised from heptane/toluene, giving 2-bromo-7-iodo-9,10-dihydrophenanthrene as colourless crystals.

1. filtration, and the precipitated product is filtered off with suction
2. washwashed with sat. sodium hydrogen-carbonate soln
3. dry with materialand dried over sodium sulfate
4. customThe solvent is removed in vacuo
5. customthe residue is recrystallised from heptane/toluene