HRID1781843

反应详情

EQUATION

反应方程式

HRID 1781843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customAfter evaporation of the methanol
  2. additionthe residue is diluted with ice-water
  3. extractionextracted twice with 400 ml of ethyl acetate each time
  4. washThe organic phases are washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue is recrystallized from methylene chloride/petroleum ether