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With copper(l) iodide; dichloro(1,1'-bis(diphenylphosphanyl)ferrocene)palladium(II)*CH2Cl2; N-ethyl-N,N-diisopropylamine In N,N-dimethyl-formamide at 100℃; for 1h; Inert atmosphere;
I Step I: Compound 162 crude
Step I: Compound 162 crude A mixture of 2,7-dibromospiro[fluorene-9,4'-tetrahydropyran] (12.00 g, 30.45 mmol) and Intermediate M (16.02 g, 85.14 mmol) in DMF (168.0 mL) is degased for 5 minutes by bubbling nitrogen in the reaction mixture. Pd(dppf)Cl2- CH2CI2 (1.680 g, 2.296 mmol) and Cul (1.685 g, 8.849 mmol are added and nitrogen is bubbled one more time in the reaction mixtures for 5 minutes. Diisopropyl ethyl amine (42.0 mL, 241 mmol) is then added and the final mixture is stirred under nitrogen atmosphere at 100°C for lh. The resulting reaction mixture is cooled to 35°C and water (336.0 mL) is added dropwise. The resulting deep red mixture is stirred overnight at RT and the resulting precipitate is filtered (MLl), washed with 100 ml of water. The resulting crude orange solid is transferred in a 250 ml RBF and triturated in 60 ml of ethanol for 30 minutes. The resulting solid is isolated by filtration and dried in a vacuum oven overnight at 45°C. To further purify the title compound, the latter is per-acetylated (Step 2), submitted to flash chromatography and de-acetylated (Step 3).
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