HRID1992312

反应详情

EQUATION

反应方程式

HRID 1992312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux overnight
  3. customwas removed under reduced pressure
  4. dissolutionThe residue was dissolved in excess of water
  5. filtrationThe resulting precipitate was filtered
  6. washwashed with water