تفاعل #2286370

معادلة التفاعل

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

methylamine

→

desired product

المردود 50.2%

N-(1-methylcarbamoyl-ethyl)nicotinamide

المردود 50.2%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvents were removed in vacuo
2. 2
   أخرىthe residue was recrystallized from hot ethyl acetate and hexanes
3. 3
   أخرىThe yellow crystals thus obtained
4. 4
   غسيلwere washed with cold ethyl acetate
5. 5
   أخرىdried

الإجراء التجريبي

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).

المصدر