N-(3-甲基丁-2-基)-3-氧代丁酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of N-(3-methylbutan-2-yl)-3-oxobutanamide obtained in Step A (500 mg) in N,N-dimethylformamide (6.0 mL) was added dropwise 1,1-dimethoxy-N,N-dimethylmethanamine (696 mg) over 5 min at room temperature, and the reaction mixture was stirred overnight at room temperature. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (methanol/ethyl acetate) to give the title compound (630 mg). The solvent was evaporated under reduced pressure the residue was purified by silica gel column chromatography (methanol/ethyl acetate)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a mixture of 3-methylbutan-2-amine (1.00 g), 2,2,6-trimethyl-4H-1,3-didioxin-4-one (2.12 g) and tetrahydrofuran (3.0 mL) was added sodium acetate (941 mg) at room temperature. The reaction mixture was refluxed overnight, and cooled to room temperature. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.46 g). The reaction mixture was refluxed overnight the mixture was extracted with ethyl acetate The extract was washed with saturated brine dried over anhydrous sodium sulfate the solvent was evaporated under reduced pressure The residue was purified by silica gel column chromatography (ethyl acetate/hexane)