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三氟甲基引入2018-11-26

Case study:

Three parrelled reactions. A mixture of 35-4000-02 (900 g, 1.8 mol, 1.0 eq), FSO2CF3COOCH3(864 g, 4.5 mol, 2.5 eq), HMPA(483 g, 2.7 mol, 1.5 eq) and CuI (855 g, 4.5 mol, 2.5 eq) in DMF (6 L) was heated at 85 oC for 16 h at N2 atmosphere. Three batches combined. The mixture was filtered to remove the insoluble solid. The filtrate was diluted with 30 kg EA. The organic layer was washed (water, 10 kg*3, brine, 10 kg*1), dried (MgSO4,3 kg), filtered and concentrated. The residue was triturated with EtOH (4 kg) to give TM (1.62 kg) as white solid.

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