methyl 2-[(3-nitropyridin-2-yl)amino]acetate synthesis
- Product Name:methyl 2-[(3-nitropyridin-2-yl)amino]acetate
- CAS Number:57461-53-7
- Molecular formula:C8H9N3O4
- Molecular Weight:211.17
Yield:57461-53-7 2.25 g
Reaction Conditions:
with triethylamine in N,N-dimethyl-formamide at 80;
Steps:
1.A A)
methyl N-(3-nitropyridin-2-yl)glycinate
A)
methyl N-(3-nitropyridin-2-yl)glycinate
To a solution of methyl glycinate hydrochloride (1.98 g) and 2-chloro-3-nitropyridine (2.50 g) in N,N-dimethylformamide (16.0 mL) was added triethylamine (5.50 mL).
The reaction mixture was stirred overnight at 80°C, and the solvent was evaporated under reduced pressure.
The residue was dissolved in ethyl acetate, the ethyl acetate solution was washed successively with water and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure.
The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.25 g).
MS (API+): [M+H]+ 212.0.
References:
EP2848618,2015,A1 Location in patent:Paragraph 0515
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