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
To a solution of 2-(4,4-dimethyl-6-(trifluoromethyl)-1,2,3,4-tetrahydroquinolin-2-yl)aniline (150 mg, 0.47 mmol) and pyridine (148 mg, 1.44 mmol) in anhydrous dichloromethane (5 mL) was added a solution of 3-fluorobenzene-1-sulfonyl chloride (92 mg, 0.36 mmol) at ice-bath. After addition, the resulting mixture was stirred at room temperature for 3 h. The reaction mixture was diluted with water, and extracted with dichloromethane. 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]-3-fluoro-benzenesulfonamide LC/MS m/e obsd. (ESI+) [(M+H)+] 478.90.
WORKUP
后处理
- additionAfter addition
- extractionextracted with dichloromethane
- dry with materialThe combined organic layer was dried over anhydrous Sodium sulfate
- concentrationconcentrated
- customThe residue was purified by HPLC