HRID985904

反应详情

EQUATION

反应方程式

HRID 985904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A pre-mix of 125 g of 30% by weight sodium hydroxide solution, 5 g of potassium iodide, 10 g of tetradecyltrimethylammonium bromide, 200 ml of tetrahydrofuran and 200 ml of toluene was heated to 75° C. A mixture of 155 g of 3,5-dimethylbenzyl chloride, 110 g of isobutyraldehyde, 50 ml of tetrahydrofuran and 50 ml of toluene was added dropwise to this pre-mix while stirring vigorously. The entire mixture was then boiled under reflux for 6 hours. The phases were then separated and the organic phase was first washed with warm water and then filtered with the addition of activated carbon. Finally, distillation was carried out using a packed column with wire spirals. The distillation, carried out in a temperature range of from 72° C. to 74° C. at 0.25 mbar, yielded 106 g of 92% 2,2-dimethyl-3-(3,5-dimethylphenyl)-propionaldehyde.

WORKUP

后处理

  1. additionwas added dropwise to
  2. additionthis pre-mix
  3. temperatureunder reflux for 6 hours
  4. customThe phases were then separated
  5. washthe organic phase was first washed with warm water
  6. filtrationfiltered with the addition of activated carbon
  7. distillationFinally, distillation
  8. distillationThe distillation
  9. customcarried out in a temperature range of from 72° C. to 74° C. at 0.25 mbar