HRID1244039

反应详情

EQUATION

反应方程式

HRID 1244039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 860 mg (4.0 mmol) N-(4-methoxy-2-methyl-phenyl)-methanesulfonamide in 15 ml DMF at ambient temperature was added 192 mg (48 mmol) 60% sodium hydride dispersion and the resulting mixture was treated with 1.14 gm, 0.5 ml (8.0 mmol) methyl iodide. The reaction mixture was stirred at room temperature for 2 hours and 0.5 ml of methyl iodide was introduced and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was diluted with 1N HCl and then extracted with ethyl acetate. The organics were washed with brine, dried with sodium sulfate and then evaporated in vacuo to afford 293 mg (X %) of a light purple solid. Mass spectrum APCI (m/z) 230 (p+1).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred at room temperature for 16 hours
  2. extractionextracted with ethyl acetate
  3. washThe organics were washed with brine
  4. dry with materialdried with sodium sulfate
  5. customevaporated in vacuo
  6. customto afford 293 mg (X %) of a light purple solid