HRID131321
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
Heat a solution of 2-(4-fluoro-2-nitro-phenylamino)-5-methyl-benzonitrile (1.747 g, 6.44 mmol) in ethanol (35 ml) to 60° C. Add a solution of tin (II) chloride (6.06 g, 31.96 mmol) in 5.0 N hydrochloric acid (35 ml) and heat the resulting mixture to reflux for 40 hours. Cool the reaction to room temperature and place in a freezer for 16 hours. Collect by filtration the product precipitates from the solution to obtain 1.3 g of the title compound (4.68 mmol, 73% yield) as a yellow-green amorphous solid: Mass Spectrum (m/e): 241(M+1).
WORKUP
后处理
- temperatureheat the resulting mixture
- temperatureto reflux for 40 hours
- temperatureCool
- customthe reaction to room temperature
- filtrationCollect by filtration the product
- customprecipitates from the solution