تفاعل #620477

معادلة التفاعل

[(5-fluoropyridine-3-carbonyl)-amino]-acetic acid methyl ester

methylamine

→

material

المردود 72.0%

5-fluoro-N-methylcarbamoylmethyl-nicotinamide

المردود 72.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىwas then immediately put onto a 55° C.
2. 2
   درجة الحرارةheating mantle for 10 min at which time the product
3. 3
   أخرىhad precipitated out of solution
4. 4
   ترشيحThe mixture was filtered in vacuo
5. 5
   غسيلthe precipitate was washed with ethanol
6. 6
   تركيزThe filtrate was concentrated
7. 7
   أخرىrecrystallized from hot ethanol

الإجراء التجريبي

To a solution of [(5-fluoropyridine-3-carbonyl)-amino]-acetic acid methyl ester (2.96 g, 14.0 mmol) in ethanol (15 mL) was added methylamine (1.5 g, 33 wt % solution in ethanol, 70 mmol). This clear solution was then immediately put onto a 55° C. heating mantle for 10 min at which time the product had precipitated out of solution. The mixture was filtered in vacuo and the precipitate was washed with ethanol. The filtrate was concentrated and recrystallized from hot ethanol. This process was repeated again to give a white fluffy material (2.11 g, 72%): mp 201-202° C.; 1H NMR (300 MHz, DMSO-d6) δ 9.10 (m, 1H), 8.93 (s, 1H), 8.76 (d, J=2.5 Hz, 1H), 8.10 (m, 1H), 7.95 (br s, 1H), 3.86 (d, J=5.8 Hz, 2H), 2.61 (d, J=4.4 Hz, 3H); ESIMS m/z 212 (M+1), m/z 210 (M−1).

المصدر