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note
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General procedure for dimerization/reduction of 1a: In a 5-mL round-bottomed flask were placed allene 1 (70.2 mg, 0.821 mmol) and tetrakis(triphenylphosphine)palladium(0) (10.3 mg, 0.0088 mmol). Dry DMF(1.5 mL) was added to the above mixture by a syringe under argon atmosphere. And then formic acid (39 μL, 0.992 mmol) was added to the reaction mixture by a microsyringe at 0 °C. The reaction mixture was stirred for 12 h in a preheated 30 °C oil bath. Then extractive work-up and solvent evaporation under reduced pressure gave the crude products which were purified on flash column chromatography (eluent: hexane/ethyl acetate (1:1)) to give a 1: 1 mixture of 2a and 3a (overall 33.4 mg, 48%) as colorless oil.
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