HRID1111282

反应详情

EQUATION

反应方程式

HRID 1111282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 1.6 M solution of butyl lithium (90.6 ml, 0.145 mol) was placed in a flask and blanketed with nitrogen and to this was added with stirring, while maintaining the temperature at 25°-30° C., 16.85 g, (0.145 mol) of tetramethylethylenediamine. The mixture was then cooled to 0° C. and 20.0 g (0.145 mol) of methoxymethoxybenzene was added with stirring and allowed to react for 2 hours after which 10.0 g (0.066 mol) of 2-hydroxy-3-methoxybenzaldehyde was added under the same conditions. The mixture was allowed to react for a few minutes and was then poured into a mixture of ice and saturated aqueous ammonium chloride. The solid that formed, which was insoluble in ether, was collected by filtration to obtain 15.5 g (81 percent of theory) of the title compound. The proton nmr spectrum was consistent with the assigned structure.

WORKUP

后处理

  1. additionto this was added
  2. temperaturewhile maintaining the temperature at 25°-30° C.
  3. stirringwith stirring
  4. additionwas added under the same conditions
  5. customto react for a few minutes
  6. customThe solid that formed
  7. filtrationwas collected by filtration