HRID34879

反应详情

EQUATION

反应方程式

HRID 34879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a suspension of 3.8 g of potassium t-butoxide in 60 ml of dry DMF under a N2 atmosphere was added portionwise 6 g of the product of Example 10 while maintaining the reaction temperature at 10°-20° C. with external cooling. After stirring at 25° C. for one hour, 9.6 g of methyl iodide was added dropwise at 10°-20° C. with external cooling. After stirring at room temperature for 16 hours, the suspension was poured into excess ice-water and filtered. The residue was recrystallized from 2-propanol to yield 4.6 g of the subject compound; m.p. 160°-162° C.

WORKUP

后处理

  1. temperaturewhile maintaining the reaction temperature at 10°-20° C. with external cooling
  2. stirringAfter stirring at room temperature for 16 hours
  3. filtrationfiltered
  4. customThe residue was recrystallized from 2-propanol