tert-butyl 2-methyl-3-oxobutanoate

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: Methyl iodide (6.86 mL, 1.1 eq) and K2CO3 (17.97 g, 1.3 eq) were added to an acetone (400 mL) solution of tert-butyl 3-oxobutanoate (15.82 g, 100 mmol) at room temperature. After 15 h, the mixture was filtered and the filtrate was concentrated. The residue was dissolved in ethyl acetate (300 mL), washed with water (30 mL) and brine (300 mL), dried (MgSO4) and concentrated. The crude residue was purified by silica gel chromatography (5-10% EtOAc-hexanes) to give tert-butyl 2-methyl-3-oxobutanoate as a colorless oil (9.56 g, 56%). MS found: (M+Na)+=195. the mixture was filtered the filtrate was concentrated The residue was dissolved in ethyl acetate (300 mL) washed with water (30 mL) and brine (300 mL) dried (MgSO4) concentrated The crude residue was purified by silica gel chromatography (5-10% EtOAc-hexanes)