HRID1036927
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-(4,4-dimethyl-6-(trifluoromethyl)-1,2,3,4-tetrahydroquinolin-2-yl)aniline (150 mg) and pyridine (1 mL) in anhydrous dichloromethane (3 mL) was added methanesulfonyl chloride (36 μL) at ice-bath under nitrogen. After addition, the resulting mixture was stirred at room temperature for 3 h. The reaction mixture was diluted with water, and extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate, concentrated. The residue was purified by HPLC to give N-[2-(4,4-dimethyl-6-trifluoromethyl-1,2,3,4-tetrahydro-quinolin-2-yl)-phenyl]-methanesulfonamide LC/MS m/e obsd. (ESI+) [(M+H)+] 399.6.
WORKUP
后处理
- additionAfter addition
- extractionextracted with ethyl acetate
- dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe residue was purified by HPLC