反应 #3404758
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08716470B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2-(Hydroxymethyl)pyrrolidine (500 mg) was mixed with dichloromethane (5 ml), and TEA (0.9 ml) and acetyl chloride (407 mg) were added thereto at 0° C., followed by stirring at room temperature overnight. 8 M Potassium hydroxide was added to the reaction mixture, followed by stirring at room temperature for 1 hour. The reaction mixture was extracted by the addition of water and CHCl3/MeOH (4:1), the organic layer was washed with water and saturated brine, and dried over anhydrous Na2SO4, and the solvent was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (MeOH/CHCl3) to obtain 1-[2-(hydroxymethyl)pyrrolidin-1-yl]ethanone (442 mg). were added at 0° C. by stirring at room temperature for 1 hour The reaction mixture was extracted by the addition of water and CHCl3/MeOH (4:1) the organic layer was washed with water and saturated brine dried over anhydrous Na2SO4 the solvent was concentrated under reduced pressure The obtained residue was purified by silica gel column chromatography (MeOH/CHCl3)
来源 ID: ord-79053b708b2d43bbbcdcaa41981c0e39