HRID486373

反应详情

EQUATION

反应方程式

HRID 486373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

41.2 g (0.271 mol) of isovanillin was dissolved in 160 ml of 90% AcOH under heating. 29.41 g of t-BuOCl was added dropwise to the solution while it was kept at 35° to 40° C. The solution was stirred at room temperature for 3 hours and then 200 ml of ether was added thereto. The mixture was left to stand overnight and crystals thus formed were separated by filtration and washed with ether. 42.0 g of the crude crystals were recrystallized from acetonitrile to obtain 35 g of 2-chloro-3-hydroxy-4-methoxybenzaldehyde (69%).

WORKUP

后处理

  1. temperatureunder heating
  2. customwas kept at 35° to 40° C
  3. waitThe mixture was left
  4. waitto stand overnight
  5. customcrystals thus formed
  6. customwere separated by filtration
  7. washwashed with ether
  8. custom42.0 g of the crude crystals were recrystallized from acetonitrile