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| 13.0g (46mmol) of 7 with 44.5g (0.25mol) of NBS and a catalytical amount of dibenzoyl peroxide ( ca. 2g in several portions) in 500ml CCl4 were heated under reflux for 4 days. After filtration of the precipitated succinimide and distillation of the solvent, the residue was crystallized from ethylmethyl ketone. A second crop of the product was obtained through concentration of the mother liquid. Yield 16.8 g (61%). For analytical and spectroscopic data, see Literature(10). |
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