3-溴-2-(溴甲基)-N,N-二甲基丙-1-胺

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of N,N-dimethyl-3-bromo-2-(bromomethyl) proprionic amide (44 g) in CH2Cl2 (300 mL) was added DIBAL (450 mL, 1.0 M in toluene) at −40° C. over 30 minutes. The mixture was allowed to warm to −10° C. over 3 hours and the diluted with CH2Cl2 (1500 mL). The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C., followed by stirring at a temperature less that 10° C. for 2 hours. The suspension was filtered, dried, and concentrated to ca. 300 mL. The product crystallized upon standing overnight at room temperature. The crystals were separated from the solution and dried (19 g, 66%). MS(M+1): 178. The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C. The suspension was filtered dried concentrated to ca. 300 mL The product crystallized upon standing overnight at room temperature The crystals were separated from the solution dried (19 g, 66%)

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of N,N-dimethyl-3-bromo-2-(bromomethyl) proprionic amide (44 g) in CH2Cl2 (300 mL) was added DIBAL (450 mL, 1.0 M in toluene) at −40° C. over 30 minutes. The mixture was allowed to warm to −10° C. over 3 hours and the diluted with CH2Cl2 (1500 mL). The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C., followed by stirring at a temperature less that 10° C. for 2 hours. The suspension was filtered, dried, and concentrated to ca. 300 mL. The product crystallized upon standing overnight at room temperature. The crystals were separated from the solution and dried (19 g, 66%). MS(M+1): 178. The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C. The suspension was filtered dried concentrated to ca. 300 mL The product crystallized upon standing overnight at room temperature The crystals were separated from the solution dried (19 g, 66%)

反应条件: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of N,N-dimethyl-3-bromo-2-(bromomethyl) proprionic amide (44 g) in CH2Cl2 (300 mL) was added DIBAL (450 mL, 1.0 M in toluene) at −40° C. over 30 minutes. The mixture was allowed to warm to −10° C. over 3 hours and the diluted with CH2Cl2 (1500 mL). The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C., followed by stirring at a temperature less that 10° C. for 2 hours. The suspension was filtered, dried, and concentrated to ca. 300 mL. The product crystallized upon standing overnight at room temperature. The crystals were separated from the solution and dried (19 g, 66%). MS(M+1): 178. The reaction was quenched with a mixture of water (300 mL) and methanol (100 mL) at −10° C. The suspension was filtered dried concentrated to ca. 300 mL The product crystallized upon standing overnight at room temperature The crystals were separated from the solution dried (19 g, 66%)