HRID629195
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 cooled (0° C.) solution of N-(2-nitrophenyl)methanesulfonamide (50 mg, 0.231 mmol) in DMF (2 mL) was added sodium hydride (11 mg, 0.46 mmol) and the reaction was warmed to room temperature and stirred for 20 minutes. The reaction was then re-cooled to 0° C. and iodomethane (0.029 mL 0.46 mmol) was added. The reaction was warmed to room temperature and stirred for 3 hours. The crude reaction was concentrated and purified by silica gel chromatography to provide N-methyl-N-(2-nitrophenyl)methanesulfonamide (20 mg, 38% yield). 1H NMR (300 MHz, CDCl3) δ 7.91 (m, 1H), 7.70-7.50 (m, 3H), 3.34 (s, 3H), 3.01 (s, 3H).
WORKUP
后处理
- temperatureThe reaction was then re-cooled to 0° C.
- temperatureThe reaction was warmed to room temperature
- stirringstirred for 3 hours
- customThe crude reaction
- concentrationwas concentrated
- custompurified by silica gel chromatography