HRID496577

反应详情

EQUATION

反应方程式

HRID 496577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 22.5 mL (0.045 mol) of a 2M solution of methylamine in dichloromethane, cooled to 0° C., was added a solution of 3.67 g (0.015 mol) of 4-but-2-ynyloxy-benzenesulfonyl chloride in 45 mL of dichloromethane. The reaction was allowed to warm to room temperature and stirred for 48 h. The resulting solution was poured into water and extracted with dichloromethane. The combined organics were washed with 2N citric acid solution, water and brine, dried over Na2SO4, filtered through Magnesol® and concentrated in vacuo to provide 3.23 g (92%) of the N-methyl sulfonamide as a white solid; m.p.78-80° C.

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. washThe combined organics were washed with 2N citric acid solution, water and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered through Magnesol®
  5. concentrationconcentrated in vacuo