HRID626318

反应详情

EQUATION

反应方程式

HRID 626318 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

1.97 g of Bis(2-methoxyethyl) azodicarboxylate was added to a mixture of 1.08 g of 2,5-dimethyl-4-nitrophenol, 0.83 g of (2,2,3,3-tetramethylcyclopropyl)methanol, 2.04 g of triphenylphosphine and 100 mL of toluene at 0° C., and the mixture was stirred at 90° C. for 4 hours. After cooling, a saturated aqueous sodium bicarbonate solution was added, and the mixture was extracted with ethyl acetate, and then the organic layer was washed with water and saturated salt water and dried over anhydrous magnesium sulfate. The resulting residue was subjected to silica gel column chromatography to obtain 0.15 g of 2,5-dimethyl-4-nitro-1-[(2,2,3,3-tetramethylcyclopropyl) methoxy]benzene.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washthe organic layer was washed with water and saturated salt water
  4. dry with materialdried over anhydrous magnesium sulfate