HRID2289677
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting solution was heated
- temperatureto reflux for 6 hours
- concentrationconcentrated
- customto give a brown oil
- customQuenched with 200 g ice
- extractionextracted with ethyl acetate
- dry with materialThe organic solution was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto give a tan solid