HRID2289677

反应详情

EQUATION

反应方程式

HRID 2289677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Chlorosulfonyl isocyanate (2.12 mL, 24.3 mmol) was added slowly to a warm solution of 3,5-diisopropyl-4-hydroxy-benzoic acid methyl ester (5.47 g, 23.1 mmol) in 300 mL toluene. The resulting solution was heated to reflux for 6 hours and then cooled to room temperature and concentrated to give a brown oil. Quenched with 200 g ice and extracted with ethyl acetate. The organic solution was dried over magnesium sulfate, filtered, and concentrated to give a tan solid. Chromatography on silica gel (20% ethyl acetate/hexanes) gave 3.58 g of the title compound as an off-white solid.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 6 hours
  3. concentrationconcentrated
  4. customto give a brown oil
  5. customQuenched with 200 g ice
  6. extractionextracted with ethyl acetate
  7. dry with materialThe organic solution was dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give a tan solid