2,2,2-triphenylethanol

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of LAH (3.9 g, 0.104 mol) in dry THF (200 mL) was stirred at 0° C. for 20 min. A solution of 2,2,2-triphenylacetic acid (10 g, 0.034 mol) in dry THF (50 mL) was added in a drop-wise manner. The reaction mixture was stirred at RT overnight. Excess LAH was quenched with 1.5 N HCl and the reaction mixture was further stirred for 2 h at RT. The reaction mixture was filtered through celite, washed with ethyl acetate and the filtrate was concentrated under vacuum. The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether) to give the title compound (4.6 g, 48%). TLC: Pet. ether/EtOAc, 7:3, Rf=0.2 The reaction mixture was stirred at RT overnight Excess LAH was quenched with 1.5 N HCl the reaction mixture was further stirred for 2 h at RT The reaction mixture was filtered through celite washed with ethyl acetate the filtrate was concentrated under vacuum The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of LAH (3.9 g, 0.104 mol) in dry THF (200 mL) was stirred at 0° C. for 20 min. A solution of 2,2,2-triphenylacetic acid (10 g, 0.034 mol) in dry THF (50 mL) was added in a drop-wise manner. The reaction mixture was stirred at RT overnight. Excess LAH was quenched with 1.5 N HCl and the reaction mixture was further stirred for 2 h at RT. The reaction mixture was filtered through celite, washed with ethyl acetate and the filtrate was concentrated under vacuum. The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet ether) to give the title compound (4.6 g, 48%). TLC: Pet. ether/EtOAc, 7:3, Rf=0.2 The reaction mixture was stirred at RT overnight Excess LAH was quenched with 1.5 N HCl the reaction mixture was further stirred for 2 h at RT The reaction mixture was filtered through celite washed with ethyl acetate the filtrate was concentrated under vacuum The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet ether)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of LAH (3.9 g, 0.104 mol) in dry THF (200 mL) was stirred at 0° C. for 20 min. A solution of 2,2,2-triphenylacetic acid (10 g, 0.034 mol) in dry THF (50 mL) was added in a drop-wise manner. The reaction mixture was stirred at RT overnight. Excess LAH was quenched with 1.5 N HCl and the reaction mixture was further stirred for 2 h at RT. The reaction mixture was filtered through celite, washed with ethyl acetate and the filtrate was concentrated under vacuum. The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether) to give the title compound (4.6 g, 48%). TLC: Pet. ether/EtOAc, 7:3, Rf=0.2 The reaction mixture was stirred at RT overnight Excess LAH was quenched with 1.5 N HCl the reaction mixture was further stirred for 2 h at RT The reaction mixture was filtered through celite washed with ethyl acetate the filtrate was concentrated under vacuum The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a suspension of LAH (3.9 g, 0.104 mol) in dry THF (200 mL) was stirred at 0° C. for 20 min. A solution of 2,2,2-triphenylacetic acid (10 g, 0.034 mol) in dry THF (50 mL) was added in a drop-wise manner. The reaction mixture was stirred at RT overnight. Excess LAH was quenched with 1.5 N HCl and the reaction mixture was further stirred for 2 h at RT. The reaction mixture was filtered through celite, washed with ethyl acetate and the filtrate was concentrated under vacuum. The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether) to give the title compound (4.6 g, 48%). TLC: Pet. ether/EtOAc, 7:3, Rf=0.2 The reaction mixture was stirred at RT overnight Excess LAH was quenched with 1.5 N HCl the reaction mixture was further stirred for 2 h at RT The reaction mixture was filtered through celite washed with ethyl acetate the filtrate was concentrated under vacuum The crude product was purified by column chromatography on silica gel (4% ethyl acetate in pet. ether)