2-(hydroxymethyl)prop-2-enoic acid

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

実験手順: To a solution of 2-(hydroxymethyl)acrylic acid (520 mg) in DMF (5.0 mL) were added tert-butyldiphenylsilyl chloride (1.65 g) and imidazole (680 mg) and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution and brine, dried over magnesium sulfate, and concentrated in vacuum condition. The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=20:1→9:1) to give the title compound (1.35 g) having the following physical data. extracted with ethyl acetate The organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution and brine dried over magnesium sulfate concentrated in vacuum condition The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=20:1→9:1)

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

実験手順: To a solution of 2-(hydroxymethyl)acrylic acid (520 mg) in DMF (5.0 mL) were added tert-butyldiphenylsilyl chloride (1.65 g) and imidazole (680 mg) and the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into 1N hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution and brine, dried over magnesium sulfate, and concentrated in vacuum condition. The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=20:1→9:1) to give the title compound (1.35 g) having the following physical data. extracted with ethyl acetate The organic layer was washed with an aqueous saturated sodium hydrogen carbonate solution and brine dried over magnesium sulfate concentrated in vacuum condition The obtained residue was purified by column chromatography on silica gel (hexane:ethyl acetate=20:1→9:1)