HRID629195

反应详情

EQUATION

反应方程式

HRID 629195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction was then re-cooled to 0° C.
  2. temperatureThe reaction was warmed to room temperature
  3. stirringstirred for 3 hours
  4. customThe crude reaction
  5. concentrationwas concentrated
  6. custompurified by silica gel chromatography