N,N-Dimethyl-N-[(E)-2-(3-nitropyridin-4-yl)vinyl]amine synthesis
- Product Name:N,N-Dimethyl-N-[(E)-2-(3-nitropyridin-4-yl)vinyl]amine
- CAS Number:908847-23-4
- Molecular formula:C9H11N3O2
- Molecular Weight:193.2
Yield:908847-23-4 45%
Reaction Conditions:
in N,N-dimethyl-formamide at 120; for 13 h;
Steps:
Synthesis of (E)-N,N-dimethyl-2-(3-nitropyridine-4-yl)ethanamine[00301] To a solution of 4-methyl-3-nitropyridine (1.0 equiv.) in DMF(5.5 M) was added l ,l-dimethoxy-N,N-dimethylmethaneamine (1.0 equiv.) and the solution was allowed to stir at 120 °C for 13hrs. The reaction was cooled to room temperature, poured onto crushed ice and stirred for 5 min. The red solid was filtered and washed with cold water. The solid was recrystallized form hot MeOH to yield (E)-N,N- dimethyl-2-(3-nitropyridine-4-yl)ethanamine as the desired product in 45% yield.LC/MS (m/z): 194.0 (MH+), R, = 0.39 min.
References:
WO2012/4217,2012,A1 Location in patent:Page/Page column 148