HRID370745

反应详情

EQUATION

反应方程式

HRID 370745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

3-(3',5'-Di-tert-butyl-4'-hydroxyphenyl)-1-propanol (100 g, 0.38 mol) was dissolved in 500 ml of trifluoracetic acid. The solution was stirred at 40° C. for six hours, then poured into an ice-water mixture. The mixture was extracted with methylene chloride. The methylene chloride layer was washed with aqueous sodium carbonate and evaporated. A solution of sodium hydroxide (25 g) in 400 ml of methanol was added to the residue. The mixture was stirred at room temperature for 30 minutes, neutralized with 1N hydrochloric acid and extracted with methylene chloride. The methylene chloride layer was washed with aqueous sodium carbonate and water, dried with anhydrous potassium carbonate, and evaporated. The residue was vacuum distilled to give 51 g (64%) of the product.

WORKUP

后处理

  1. extractionThe mixture was extracted with methylene chloride
  2. washThe methylene chloride layer was washed with aqueous sodium carbonate
  3. customevaporated
  4. additionA solution of sodium hydroxide (25 g) in 400 ml of methanol was added to the residue
  5. stirringThe mixture was stirred at room temperature for 30 minutes
  6. extractionextracted with methylene chloride
  7. washThe methylene chloride layer was washed with aqueous sodium carbonate and water
  8. dry with materialdried with anhydrous potassium carbonate
  9. customevaporated
  10. distillationdistilled