HRID490328

反应详情

EQUATION

反应方程式

HRID 490328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

To a solution of ethyl 3,5-dimethyl-2-pyrrolecarboxylate (Aldrich) (504 mg, 3 mmol) in THF/H2O/MeOH (5:1:1, 30 ml) was added NaOH (480 mg, 12 mmol) in H2O (12 ml). The mixture was stirred at 75° C. overnight. The homogeneous mixture was washed with ether. To the aqueous layer was added a saturated aqueous KHSO4 solution until the pH was about 3. The solution was then extracted with dichloromethane. The extracts were dried over MgSO4 and evaporated. The residue was purified on silica (ethylacetate/methanol 90/10) to give the title compound (375 mg, 90%).

WORKUP

后处理

  1. washThe homogeneous mixture was washed with ether
  2. additionTo the aqueous layer was added a saturated aqueous KHSO4 solution until the pH was about 3
  3. extractionThe solution was then extracted with dichloromethane
  4. dry with materialThe extracts were dried over MgSO4
  5. customevaporated
  6. customThe residue was purified on silica (ethylacetate/methanol 90/10)