反应 #2286371

反应方程式

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

methylamine

→

material

收率 72.0%

5-fluoro-N-methylcarbamoylmethyl-nicotinamide

收率 72.0%

溶剂

ethanol

反应条件

后处理

1. 1
   其他was then immediately put onto a 55° C.
2. 2
   温度heating mantle for 10 min at which time the product
3. 3
   其他had precipitated out of solution
4. 4
   过滤The mixture was filtered in vacuo
5. 5
   洗涤the precipitate was washed with ethanol
6. 6
   浓缩The filtrate was concentrated
7. 7
   其他recrystallized from hot ethanol

实验过程

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).

来源