HRID1781843
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
35.8 g of 2-chloro-3-formyl-6-methoxy-5-nitrophenyl acetate are dissolved in 300 ml of methanol. After adding 145 ml of 1N sodium hydroxide solution the mixture is stirred at 23° for 1 hour. After evaporation of the methanol, the residue is diluted with ice-water, made acid with 2N hydrochloric acid and extracted twice with 400 ml of ethyl acetate each time. The organic phases are washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. The residue is recrystallized from methylene chloride/petroleum ether. There is obtained 2-chloro-3-hydroxy-5-nitro-p-anisaldehyde of m.p. 130°.
WORKUP
后处理
- customAfter evaporation of the methanol
- additionthe residue is diluted with ice-water
- extractionextracted twice with 400 ml of ethyl acetate each time
- washThe organic phases are washed with saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- customevaporated
- customThe residue is recrystallized from methylene chloride/petroleum ether