HRID2221152

反应详情

EQUATION

反应方程式

HRID 2221152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Suspend sodium hydride (310 mg, 13 mmol) in a solution of ethylene glycol (800 mg, 13 mmol) in DMF (50 mL) previously cooled to 0° C. Allow the mixture to warm to room temperature and stir for 30 min. Add 7-bromo-2-chloroquinoxaline (610 mg, 2.5 mmol) and stir the resulting mixture for 2 h at room temperature. Dilute the mixture with 3:1 chloroform/isopropyl alcohol and wash the resulting solution with saturated sodium chloride solution. Dry and concentrate the organic phase in vacuo and purify the residue via silica gel chromatography to provide 564 mg (85%) of the titled compound. MS ES+ m/e 268 (M+1). 1H NMR (400 MHz, CDCl3) δ 8. (s, 1H), 8.0 (d, J=2.0 Hz, 1H), 7.90 (dd, J=8.8, 2.0 Hz, 1H), 7.7 (d, J=8.8 Hz, 1H), 4.6 (t, J=4.8 Hz, 2H), 4.39 (t, J=4.8 Hz, 2H).

WORKUP

后处理

  1. temperatureAllow the mixture to warm to room temperature
  2. washwash the resulting solution with saturated sodium chloride solution
  3. customDry
  4. concentrationconcentrate the organic phase in vacuo
  5. custompurify the residue via silica gel chromatography