HRID2284400

反应详情

EQUATION

反应方程式

HRID 2284400 的结构方程式

PROCEDURE

实验过程

To a 100 mL round bottom flask, 3-amino-5-bromo-pyridine-2-carboxylic acid amide (1.05 g, 0.0049 mol) and aqueous sodium hydroxide solution (0.98 g in 10 mL water, 0.0245 mol) were added. The reaction mixture was stirred at reflux temperature for 5 hours. The volatiles were evaporated under reduced pressure to provide the residue. The residue was neutralized to pH 7.0, using 2N HCl at 0° C. to obtain the precipitate. The precipitate was filtered and dried to provide the title compound as light yellow solid (1 g, 95%). 1H NMR (300 MHz, DMSO-d6): δ 7.65 (d, J=2.1 Hz, 1H), 7.20 (d, J=2.1 Hz, 1H), 7.01-7.16 (br s, 2H); LC-MS (ESI): Calculated mass: 216.0; Observed mass [M+H]+: 217.0. (RT: 0.43 min).

WORKUP

后处理

  1. temperatureat reflux temperature for 5 hours
  2. customThe volatiles were evaporated under reduced pressure
  3. customto provide the residue
  4. customat 0° C.
  5. customto obtain the precipitate
  6. filtrationThe precipitate was filtered
  7. customdried