HRID867983

反应详情

EQUATION

反应方程式

HRID 867983 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To paraformaldehyde (40 g, 1.3 mole) in 100 ml isopropanol at 25° C. was added morpholine (88 ml) in 0.5 liter isopropanol. The reaction mixture was refluxed for 30 minutes to effect solution. To the solution, 4-t-octylcatechol (222 g, 1.0 mole) dissolved in 0.5 liter isopropanol was added dropwise while maintaining the solution temperature at 60° C. The reaction mixture was stirred at reflux overnight. The reaction was cooled to 25° C. and the solvent was removed in vacuo to give a white solid which was triturated with 750 ml petroleum ether and collected. Overall yield from two crops was 86%, 280 g.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 30 minutes
  2. additionwas added dropwise
  3. temperatureat reflux overnight
  4. temperatureThe reaction was cooled to 25° C.
  5. customthe solvent was removed in vacuo
  6. customto give a white solid which
  7. customwas triturated with 750 ml petroleum ether
  8. customcollected
  9. customOverall yield from two crops