HRID462033

反应详情

EQUATION

反应方程式

HRID 462033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To 1 liter of dry tetrahydrofuran was added 52 g of diisopropylamine. The mixture was cooled to -78° C and 325 ml of 1.6 M n-butyllithium in hexane was added. After 1 hour of stirring 52 g of methyl isobutyrate was added dropwise followed by stirring for another 30 minutes. Then 63 g of α, α'-dibromo-p-xylene was slowly added. The reaction mixture was stirred overnight and brought to room temperature. The mixture was filtered and solvent was removed from the filtrate by evaporation. The residue was recrystallized from methanol to obtain 63 g of 1,4-bis(2-carbomethoxy-2methylpropyl)benzene, m.p. 74°-76° C.

WORKUP

后处理

  1. additionwas added dropwise
  2. stirringThe reaction mixture was stirred overnight
  3. custombrought to room temperature
  4. filtrationThe mixture was filtered
  5. customsolvent was removed from the filtrate by evaporation
  6. customThe residue was recrystallized from methanol