HRID2308869

反应详情

EQUATION

反应方程式

HRID 2308869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

120 mg of 2-(3-chloropropyl)-5-hydroxy-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 77) were dissolved in 2 ml of acetone, after which 660 mg of sodium iodide were added, and the reaction mixture was heated under reflux for 10 hours. The reaction mixture was cooled and then poured into water, and the resulting precipitate was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate. The ethyl acetate was distilled off under reduced pressure and the resulting crude product was purified in the same manner as described in (a), to give the title compound having the same Rf value and mass spectrum as the product of (a) above.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 10 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionthe resulting precipitate was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe ethyl acetate was distilled off under reduced pressure
  8. customthe resulting crude product was purified in the same manner