HRID2055181

反应详情

EQUATION

反应方程式

HRID 2055181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of dimethyl 4,4-dimethyl-cyclohexane-1,1-dicarboxylate (5.23 g, 22.9 mmol) in diethyl ether (250 mL) at −78° C. under a nitrogen atmosphere was added diisobutylaluminum hydride (1.5M in toluene, 30.6 mL, 45.9 mmol) dropwise. After 2.5 h, the reaction mixture was quenched with a mixture of methanol (75 mL) and water (75 mL). The mixture was filtered through Celite@ and the aqueous phase was extracted with diethyl ether (100 mL×5), was dried (MgSO4) and was evaporated in vacuo to yield the title compound which was used without further purification. MH+199.

WORKUP

后处理

  1. customthe reaction mixture was quenched with a mixture of methanol (75 mL) and water (75 mL)
  2. filtrationThe mixture was filtered through Celite@
  3. extractionthe aqueous phase was extracted with diethyl ether (100 mL×5)
  4. dry with materialwas dried (MgSO4)
  5. customwas evaporated in vacuo