HRID487471

反应详情

EQUATION

反应方程式

HRID 487471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

36.6 g (170 mmol) of pyridinium chlorochromate are placed at room temperature in 120 ml of dichloromethane under N2, and a solution of 20.4 g (113 mmol) of 4-benzyloxybutanol in 20 ml of dichloromethane is added. The reaction mixture rapidly becomes dark and the reaction is slightly exothermic. The reaction mixture is stirred at room temperature for 31/2 hours. The supernatant dichloromethane phase is decanted off and concentrated by evaporation in a rotary evaporator. The residue is filtered over 100 g of silica gel. The product fractions are concentrated by evaporation in a rotary evaporator and distilled under a high vacuum over a 10 cm Vigreux column. 4-benzyloxybutanal is obtained, b.p.0.1 =72°-73°.

WORKUP

后处理

  1. customThe supernatant dichloromethane phase is decanted off
  2. concentrationconcentrated by evaporation in a rotary evaporator
  3. filtrationThe residue is filtered over 100 g of silica gel
  4. concentrationThe product fractions are concentrated by evaporation in a rotary evaporator
  5. distillationdistilled under a high vacuum over a 10 cm Vigreux column