反应 #2286370

反应方程式

2-[(pyridine-3-carbonyl)-amino]-propionic acid methyl ester

methylamine

→

desired product

收率 50.2%

N-(1-methylcarbamoyl-ethyl)nicotinamide

收率 50.2%

溶剂

ethanol

反应条件

后处理

1. 1
   其他The solvents were removed in vacuo
2. 2
   其他the residue was recrystallized from hot ethyl acetate and hexanes
3. 3
   其他The yellow crystals thus obtained
4. 4
   洗涤were washed with cold ethyl acetate
5. 5
   其他dried

实验过程

To a solution of 2-[(pyridine-3-carbonyl)-amino]-propionic acid methyl ester (10.4 g, 50 mmol) in ethanol (50 mL) was added methylamine (24 g, 33 wt % solution in ethanol, 250 mmol). The reaction mixture was heated at 55° C. for 45 min. The solvents were removed in vacuo and the residue was recrystallized from hot ethyl acetate and hexanes. The yellow crystals thus obtained were washed with cold ethyl acetate and dried to give the desired product (5.2 g, 50%): 1H NMR (300 MHz, DMSO-d6) δ 9.05 (br s, 1H), 8.77-8.70 (m, 2H), 8.24 (m, 2H), 7.89 (br s, 1H), 7.50 (m, 1H), 2.59 (d, J=4.7 Hz, 3H), 1.33 (d, J=7.4 Hz, 3H); ESIMS m/z 208.1 (M+1), m/z 206.1 (M−1).

来源