HRID987366

反应详情

EQUATION

反应方程式

HRID 987366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-Isopropyl-4-nonylphenol (3a) (239.4 g, 0.914 mol) in toluene (470 mL) was placed in a 4-neck RBF equipped with a thermometer, a condenser, and a mechanical stirrer. To the solution was added methanolic magnesium methoxide (685 mL of 7.4 wt. %, d. 0.816 g/mL). The methanol was distilled off gradually so that the pot temperature was raised to 100° C. Then solid paraformaldehyde (80 g, 2.7 mol) was introduced in portions for 30 mins. maintaining the same temperature. Crude product was distilled and further purified by flash column chromatography to obtain 3-isopropyl-5-nonylsalicylaldehyde (52.6 g) in 20% yield.

WORKUP

后处理

  1. customequipped with a thermometer, a condenser, and a mechanical stirrer
  2. distillationThe methanol was distilled off gradually so that the pot temperature
  3. temperaturemaintaining the same temperature
  4. distillationCrude product was distilled
  5. customfurther purified by flash column chromatography