HRID2396554

反应详情

EQUATION

反应方程式

HRID 2396554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 2-methyl-1,4-dihydrobenzoic acid (0.085g, 0.50 mmol; 81% pure, from Aldrich Chemical Company) in decalin (5 mL) under a nitrogen atmosphere is added a polysiloxane matrix material containing a homogenous dispersion of rhodium and aluminum (0.100 g). The solution is heated to reflux for 19 hours. On cooling the reaction mixture is diluted with hexane (25 mL) and extracted with aqueous sodium hydroxide (5%) solution (2×5 mL). The basic aqueous solution is acidified and extracted with chloroform (3×4 mL). The combined organic layer is dried over anhydrous sodium sulfate. The solvent is evaporated using a rotary evaporator to give 2-methylbenzoic acid.

WORKUP

后处理

  1. temperatureThe solution is heated
  2. temperatureto reflux for 19 hours
  3. temperatureOn cooling the reaction mixture
  4. extractionextracted with aqueous sodium hydroxide (5%) solution (2×5 mL)
  5. extractionextracted with chloroform (3×4 mL)
  6. dry with materialThe combined organic layer is dried over anhydrous sodium sulfate
  7. customThe solvent is evaporated
  8. customa rotary evaporator