反応 #2286371

反応方程式

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

methylamine

→

material

収率 72.0%

5-fluoro-N-methylcarbamoylmethyl-nicotinamide

収率 72.0%

溶媒

ethanol

反応条件

後処理

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

実験手順

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).

出典