HRID325120

反应详情

EQUATION

反应方程式

HRID 325120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

110 ml of a solution of methyl magnesium bromide (3.0 M) in diethyl ether was diluted with 100 ml of anhydrous tetrahydrofuran (THF). Then, the solution was put into a 1 liter flask and then maintained at 0° C. 2-adamantanone (45 g, 0.3 mol) was dropped slowly using a dropping funnel and then the reaction was stirred at room temperature for about 12 hours. After completion of the reaction, excess THF was removed using a rotary evaporator and then the resultant product was poured into water. Then, the resultant product was neutralized with dilute sulfuric acid and extracted using diethyl ether and was then dried over magnesium sulfate. The obtained crude product was recrystallized using n-hexane and a methylene chloride cosolvent to yield the desired product 2-methyl-2-adamantanol (yield: 80%).

WORKUP

后处理

  1. customThen, the solution was put into a 1 liter flask
  2. customwas removed
  3. customa rotary evaporator
  4. additionthe resultant product was poured into water
  5. extractionextracted
  6. dry with materialwas then dried over magnesium sulfate
  7. customThe obtained crude product
  8. customwas recrystallized