HRID74145

反应详情

EQUATION

反应方程式

HRID 74145 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An eggplant flask was charged with 4-fluoro-3-nitrobenzoic acid (2.51 g, 13.56 mmol), aniline (2.52 g, 27.12 mmol), and ethanol (9.5 mL), and this was heated to reflux with stirring for 16 hours. After cooling to room temperature, the mixture was poured into dilute hydrochloric acid (1 M, 50 mL), diluted with distilled water (100 mL), was left to stir as is at room temperature for 30 minutes. The precipitated crystals were filtered off, and washed successively with dilute hydrochloric acid (1 M, with approx. 3 mL 3 times), distilled water (approx. 5 mL 2 times), and with diethyl ether (approx. 3 mL). The crystals obtained were dried at reduced pressure with heating to yield the title compound (3.39 g, quant.) as a reddish-orange solid.

WORKUP

后处理

  1. temperaturethis was heated
  2. temperatureto reflux
  3. waitwas left
  4. stirringto stir
  5. waitas is at room temperature for 30 minutes
  6. filtrationThe precipitated crystals were filtered off
  7. washwashed successively with dilute hydrochloric acid (1 M, with approx. 3 mL 3 times)
  8. distillationdistilled water (approx. 5 mL 2 times)
  9. customThe crystals obtained
  10. customwere dried at reduced pressure
  11. temperaturewith heating