反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of N-(2-phenyl-pyridin-3-yl)-acetamide hydrochloride (61.9 g, 24.9 mmol) in tetrahydrofuran (100 mL) was added concentrated hydrochloric acid (100 mL). The reaction mixture was heated to reflux overnight and concentrated to a low volume. Tetrahydrofuran was added (2000 mL) and the volume was reduced to about 1000 mL as, product started precipitating. The mixture was cooled to 0° C. and was granulated for two) hours. The solids were filtered to afford 2-phenyl-3-aminopyridine hydrochloride (46.2 g, 90%). M. p.=226-1227° C. 1H NMR (300 MHz, CDCl3) δ6.35 (bs, 3), 7.61-7.74 (m, 6), 7.82 (dd, 1, J=1.4, 8.6), 8.05 (dd, 1, J=1.5, 5.4). Analysis calculated for C11H11CIN2: C, 63.93; H, 5.36; N, 13.55. Found: C, 63.64; H, 5.20; N, 13.49.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux overnight
- concentrationconcentrated to a low volume
- additionTetrahydrofuran was added (2000 mL)
- customstarted precipitating
- filtrationThe solids were filtered