反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethis was heated
- temperatureto reflux
- waitwas left
- stirringto stir
- waitas is at room temperature for 30 minutes
- filtrationThe precipitated crystals were filtered off
- washwashed successively with dilute hydrochloric acid (1 M, with approx. 3 mL 3 times)
- distillationdistilled water (approx. 5 mL 2 times)
- customThe crystals obtained
- customwere dried at reduced pressure
- temperaturewith heating