HRID50364
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
To a solution of 25 mL of ethanol/glacial acetic acid/water (2:2:1) were added 0.6 g (2.9 mmol) of methyl 4-formyl-3-nitrobenzoate, 1.2 g (21.4 mmol) of iron powder and 0.01 mL of concentrated hydrochloric acid and the mixture was refluxed with stirring for 15 minutes. Then the iron was separated off, the solution was diluted with water and extracted with methylene chloride. The combined organic extracts were washed with water, dried, and evaporated down. Yield: 0.3 g (58% of theory); Rf value: 0.74 (silica gel, methylene chloride/methanol=9.5:0.5).
WORKUP
后处理
- temperaturethe mixture was refluxed
- customThen the iron was separated off
- additionthe solution was diluted with water
- extractionextracted with methylene chloride
- washThe combined organic extracts were washed with water
- customdried
- customevaporated down