tert-butyl N-[2-(methoxymethylamino)-2-oxoethyl]carbamate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: Isopropylmagnesium bromide (15.5 ml, 2M in THF) was added to a solution of 3-bromopyridine (4.92 g) in THF (30 ml) at 0° C. and stirred for 1 h. A solution of the product from step (a) (2.18 g) in THF (20 ml) was then added and the reaction mixture was stirred at room temperature for 40 h. The mixture was quenched by the addition of saturated ammonium chloride solution (250 ml) and extracted with ethyl acetate. The organic layer was washed with brine and dried (MgSO4). The solvent was evaporated off and the residue purified by chromatography (silica, 20% ethyl acetate/dichloromuethane as eluent) to give the sub-title compound (1.84 g) as a white solid. the reaction mixture was stirred at room temperature for 40 h The mixture was quenched by the addition of saturated ammonium chloride solution (250 ml) extracted with ethyl acetate The organic layer was washed with brine dried (MgSO4) The solvent was evaporated off the residue purified by chromatography (silica, 20% ethyl acetate/dichloromuethane as eluent)

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

実験手順: N,O-Dimethylhydroxylamine hydrochloride (1.95 g), EDCI (3.83 g), N-methylmorpholine (2.2 ml) and DMAP (2.44 g) were added to a solution of N-[(1,1-dimethylethoxy)carbonyl]glycine (3.5 g) in dichloromethane (60 ml) and then stirred at room temperature for 3 days. Dichloromethane (100 ml) was added and then the solution was washed with 2M hydrochloric acid (three times), NaHCO3 solution (three times) and water (three times) and then dried (MgSO4). The organic layer was separated and the aqueous layer was further extracted twice. The solvent was evaporated to give the sub-title compound (3.42 g). the solution was washed with 2M hydrochloric acid (three times), NaHCO3 solution (three times) and water (three times) dried (MgSO4) The organic layer was separated the aqueous layer was further extracted twice The solvent was evaporated