HRID2289687

反应详情

EQUATION

反应方程式

HRID 2289687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Chlorosulfonyl isocyanate (1.02 mL, 11.7 mmol) was added to a warm solution of 2,6-diisopropyl-4-thiocyanato-phenol (2.5 g, 10.6 mmol) in 150 mL toluene. The resulting solution was heated to reflux for 6 hours and then cooled to room temperature and stirred overnight. The reaction was concentrated in vacuo and the residue was quenched with ice water and extracted with dichloromethane. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give 1.75 g of sulfamic acid 2,6-diisopropyl-4-thiocyanato-phenyl ester as a white solid.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 6 hours
  3. concentrationThe reaction was concentrated in vacuo
  4. customthe residue was quenched with ice water
  5. extractionextracted with dichloromethane
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated