HRID1284820

反应详情

EQUATION

反应方程式

HRID 1284820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,4-dimethyl-5-(trifluoromethanesulfonamido)benzenesulfonyl chloride (1.5 g), a 40% aqueous solution of methylamine (1 g) and water (20 ml) was stirred at room temperature and allowed to stand overnight at the same temperature. The resultant mixture was made acidic with 5% aqueous hydrochloric acid to precipitate an oily substance, which was then extracted with chloroform. The organic layer was washed with a 5% aqueous solution of hydrochloric acid and water in order and dried over anhydrous magnesium sulfate, followed by concentration. The residue was allowed to stand to give crystals, which were recrystallized from toluene to give 1.1 g of N-methyl-2,4-dimethyl-5-(trifluoromethanesulfonamido)benzenesulfonamide. M.P., 134.5°-135.5° C.

WORKUP

后处理

  1. customto precipitate an oily substance, which
  2. extractionwas then extracted with chloroform
  3. washThe organic layer was washed with a 5% aqueous solution of hydrochloric acid and water in order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationfollowed by concentration
  6. customto give crystals, which
  7. customwere recrystallized from toluene