HRID1992312
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
PROCEDURE
实验过程
To a solution of 2-[(1-benzothien-2-ylcarbonyl)amino]nicotinamide (0.3 g, 1.0 mmol) in ethanol (20 mL) was added NaOH (10 N, 0.3 mL, 3.0 mmol). The resulting solution was heated to reflux overnight. On cooling to rt the solvent was removed under reduced pressure. The residue was dissolved in excess of water and acidified with HCl. The resulting precipitate was filtered and washed with water to afford the product as yellow powder (0.16 g, 57%). HPLC/MS: (M+H)+ 280.0 m/z; Retention time (LC-MS)=2.66 min; 1H NMR (DMSO-D6): 13.17 (1H, s); 8.94(1H, m); 8.61(1H, s); 8.50(1H, d); 8.08(1H, d); 7.97(1H, d); 7.52(3H, m).
WORKUP
后处理
- temperatureThe resulting solution was heated
- temperatureto reflux overnight
- customwas removed under reduced pressure
- dissolutionThe residue was dissolved in excess of water
- filtrationThe resulting precipitate was filtered
- washwashed with water