反応 #2286370

反応方程式

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

methylamine

→

desired product

収率 50.2%

N-(1-methylcarbamoyl-ethyl)nicotinamide

収率 50.2%

溶媒

ethanol

反応条件

後処理

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

実験手順

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).

出典