HRID1857401

反应详情

EQUATION

反应方程式

HRID 1857401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirred solution of 2-bromo-5-fluoro-4-nitrotoluene (1.662 g, 7.102 mmol, as prepared above) in DMF (7.0 mL) at 70° C., was added, dropwise, a solution of sodium glycinate (0.690 g, 7.11 mmol, Aldrich, used as received) in water (7.0 mL). The resulting suspension was stirred overnight at 70° C. The suspension was cooled to room temperature and the red solid was filtered, washed with acetone, and dried under vacuum to give 0.932 g (45%) of the pure (1H NMR) title compound as a red powder; 1H NMR (DMSO-d6): δ 2.306 (s, 3H), 3.452 (d, 2H, J=3.9Hz), 6.874 (s, 1H), 8.125 (s, 1H), 8.779 (s, 1H).

WORKUP

后处理

  1. temperatureThe suspension was cooled to room temperature
  2. filtrationthe red solid was filtered
  3. washwashed with acetone
  4. customdried under vacuum