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1357259-50-7

1-(3-aMino-5-broMopyridin-2-yl)ethanone hcl synthesis

5synthesis methods
Ethanone, 1-[5-bromo-3-[[(2,4-dimethoxyphenyl)methyl]amino]-2-pyridinyl]-

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1-(3-aMino-5-broMopyridin-2-yl)ethanone hcl

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Yield:1357259-50-7 99.67%

Reaction Conditions:

with trifluoroacetic acid in dichloromethane at 20; for 2 h;

Steps:

172

Trifluoroacetic acid (2.5 mL, 32.61 mmol) was added to a solution of 1-[5-bromo-3- [(2,4-dimethoxyphenyl)methylamino]pyridin-2-yl]ethanone (3.97 g, 10.87 mmol) in DCM (38 mL) and the resulting mixture was stirred at room temperature for 2 hours, after which the solvent was removed in vacuo. The resulting solid was triturated with diethyl ether, the white solid was filtered off and the filtrate washed with saturated aqueous Na2CO3 solution, dried over Na2SO4 and the solvent removed under reduced pressure to give 1-(3-amino-5- bromopyridin-2-yl)ethanone (2.33 g, 10.83 mmol, 99.67% yield) as a yellow solid.1H NMR (400 MHz, DMSO-d6) δ 2.53 (s, 3H), 7.28 (s, 2H), 7.48 (d, J = 2.07 Hz, 1H), 7.92 (d, J = 2.06 Hz, 1H). LC-MS (Method A): r.t.0.89 min, MS (ESI) m/z = 215.0 [M+H]+.

References:

WO2022/20244,2022,A1 Location in patent:Page/Page column 454

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1-(3-aMino-5-broMopyridin-2-yl)ethanone hcl

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1-(3-aMino-5-broMopyridin-2-yl)ethanone hcl

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