TERT-BUTYL N-(2-MORPHOLINO-2-OXOETHYL)CARBAMATE

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: To a stirred solution of the above (2-morpholin-4-yl-2-oxo-ethyl)-carbamic acid tert-butyl ester (0.44 g, 1.8 mmol) in 1,4-dioxane (4.0 mL), HCl (4.0 mL of a 4 M solution in 1,4-dioxane) was added at room temperature. After one h, the precipitated product was collected via filtration and washed with EtOAc. The solid was dried under high vacuum to give 0.23 g (76%) of 2-amino-1-morpholin-4-yl-ethanone hydrochloride which was used without further purification. After one h, the precipitated product was collected via filtration washed with EtOAc The solid was dried under high vacuum

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

实验步骤: To a stirred solution of N-(tert-butoxycarbonyl)glycine (3.0 g, 17.1 mmol) in DMF (75 mL), N,N-diisopropylethylamine (14.9 mL, 85.5 mmol) was added, followed by EDC (3.6 g, 18.8 mmol) and HOBT (2.5 g, 18.8 mmol) at 0° C., under argon. The resulting mixture was stirred for 0.5 h after which time morpholine (3.0 mL, 34.2 mmol) was introduced in a dropwise manner. Upon complete addition, the reaction was warmed to ambient temperature, stirred overnight and concentrated. The resulting residue was diluted with EtOAc and saturated NaHCO3. The layers were separated and the aqueous phase was extracted with EtOAc. The combined organics were dried (MgSO4), filtered and concentrated to give 2.3 g (55%) of (2-morpholin-4-yl-2-oxo-ethyl)-carbamic acid tert-butyl ester which was used without further purification. was introduced in a dropwise manner Upon complete addition concentrated The resulting residue was diluted with EtOAc and saturated NaHCO3 The layers were separated the aqueous phase was extracted with EtOAc The combined organics were dried (MgSO4) filtered concentrated