1-[6-(methylamino)-3-pyridinyl]ethanone synthesis
- Product Name:1-[6-(methylamino)-3-pyridinyl]ethanone
- CAS Number:856014-63-6
- Molecular formula:C8H10N2O
- Molecular Weight:150.18
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Yield:856014-63-6 258 mg
Reaction Conditions:
in tetrahydrofuran at 130; for 0.5 h;Microwave irradiation;
Steps:
42.1 1-(6-methylaminopyrid-3-yl)ethanone
A mixture of 2 mL of ethanol, 280 mg (1.80 mmol) of 1-(6-chloropyrid-3-yl)ethanone and 4.50 mL (9 mmol) of a 2 M solution of methylamine in THF is heated in a Biotage microwave reactor at 130°C for 30 minutes. The reaction medium is evaporated to dryness. The crude product is taken up in water and extracted with EtOAc. The organic phase is dried over magnesium sulfate and evaporated to dryness. 258 mg of 1-(6-methylaminopyrid-3-yl)ethanone are obtained, the characteristics of which are as follows: 1H NMR (300 MHz, δ in ppm, DMSO-d6): 2.42 (s, 3H), 2.84 (s, 3H), 6.47 (m, 1 H), 7.42 (m, 1 H), 7.85 (m, 1 H), 8.65 (m, 1 H).
References:
WO2013/190123,2013,A1 Location in patent:Page/Page column 121
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