HRID85008

反应详情

EQUATION

反应方程式

HRID 85008 的结构方程式

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

A mixture of 2,3,6-trimethylphenol (5 g, 0.036 mol) and hexamethylenetetramine (2.06 g, 0.0147 mol) in acetic acid (20 ml) was stirred at 115° C. for 2 hrs. The solvent (10 ml) was distilled and 20% (v/v) H2SO4 (20 ml) was added, and then the mixture was stirred at 115° C. for 20 min. The mixture was then poured on ice cold water (50 ml) and the separated solid was filtered, washed well with cold water (25 ml) and suck-dried. The wet cake was dried at 90° C. for 2 hrs under vacuum to yield 2,3,5-trimethyl-4-hydroxy-benzaldehyde (4.5 g, 75%; Table 1, no. 12).

WORKUP

后处理

  1. distillationThe solvent (10 ml) was distilled
  2. addition20% (v/v) H2SO4 (20 ml) was added
  3. stirringthe mixture was stirred at 115° C. for 20 min
  4. additionThe mixture was then poured on ice cold water (50 ml)
  5. filtrationthe separated solid was filtered
  6. washwashed well with cold water (25 ml)
  7. customsuck-dried
  8. customThe wet cake was dried at 90° C. for 2 hrs under vacuum