HRID971969

反应详情

EQUATION

反应方程式

HRID 971969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution prepared by dissolving 1.3 g of triethylamine hydrochloride (0.009 mole) in 69.2 g of a 35.8% aqueous solution of sodium bisulfite (0.238 mole of sodium bisulfite) while being stirred at room temperature, was added dropwise taking 2 hours a solution prepared by dissolving 50 g of crude 3-phenoxybenzaldehyde (72.5% purity (0.183 mole of 3-phenoxybenzaldehyde) and containing no other aldehyde compounds) in 80 g of toluene. Immediately after the starting of the dropwise addition, white crystals began to precipitate out of the reaction system. After completion of the addition, stirring was continued for a further 2 hours. The crystals were collected by filtration, washed three times with 50 g of toluene, and dried to obtain 54.5 g (98.5% yield) of 3-phenoxybenzaldehyde sodium bisulfite adduct.

WORKUP

后处理

  1. customTo a solution prepared
  2. additionwas added dropwise
  3. customa solution prepared
  4. additionImmediately after the starting of the dropwise addition, white crystals
  5. customto precipitate out of the reaction system
  6. additionAfter completion of the addition
  7. stirringstirring
  8. waitwas continued for a further 2 hours
  9. filtrationThe crystals were collected by filtration
  10. washwashed three times with 50 g of toluene
  11. customdried