反応 #73953

反応方程式

2-bromo-1-(3-nitrophenyl)ethanone

triethylamine

(2,4-dichlorophenyl)-N-methylmethanamine

→

2-((2,4-dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone

溶媒

1,4-dioxane

反応条件

後処理

1. 1
   その他Into a 100-mL 3-necked round-bottom flask purged
2. 2
   温度maintained with an inert atmosphere of nitrogen
3. 3
   濃縮The mixture was concentrated under vacuum
4. 4
   その他This resulted in 1.5 g (50%) of 2-((2,4-dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone as a yellow solid

実験手順

Into a 100-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-bromo-1-(3-nitrophenyl)ethanone (2 g, 8.23 mmol, 1.00 equiv), triethylamine (3.4 g, 4.00 equiv), (2,4-dichlorophenyl)-N-methylmethanamine (1.9 g, 10.05 mmol, 1.20 equiv), 1,4-dioxane (50 mL). The resulting solution was stirred for 2 h at room temperature at which time it was judged to be complete by LCMS. The mixture was concentrated under vacuum and the residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:100-1:50). This resulted in 1.5 g (50%) of 2-((2,4-dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone as a yellow solid.

出典