반응 #91311

반응 방정식

3-Fluoroisonicotinic acid

3-fluorobenzylamine

→

title compound

수율 33.2%

3-[(3-fluorobenzyl)amino]pyridine-4-carboxylic acid

수율 33.2%

용매

DMA

반응 조건

후처리

1. 1
   농축The solution was concentrated in vacuo
2. 2
   기타purified through a short plug of silica gel chromatography (20% MeOH/DCM)
3. 3
   농축The semi-pure fractions were concentrated
4. 4
   기타to give a white precipitate, which
5. 5
   여과was collected by filtration
6. 6
   기타dried under vacuum

실험 절차

3-Fluoroisonicotinic acid (100 mg, 0.71 mmol) and 3-fluorobenzylamine (308 μL, 2.84 mmol) were combined in DMA (3 mL) and the solution was stirred at 168° C. in a microwave for 90 min. The solution was concentrated in vacuo and purified through a short plug of silica gel chromatography (20% MeOH/DCM). The semi-pure fractions were concentrated and then taken up in water to give a white precipitate, which was collected by filtration and dried under vacuum to give 58 mg (33%) of the title compound. 1H NMR (500 MHz, DMSO-d6): δ 8.18 (s, 1H), 7.99 (br s, 1H), 7.84 (d, 1H, J=5.0 Hz), 7.58 (d, 1H, J=5.0 Hz), 7.31-7.41 (m, 2H), 7.15-7.23 (m, 2H), 4.62 (s, 2H). [M+H] calc'd for C13H11FN2O2, 247. found 247.

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