HRID35503

反应详情

EQUATION

反应方程式

HRID 35503 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-methyl-2,4-dimethyl-5-(trifluoromethanesulfonamido)benzenesulfonamide (2 g) and triethylamine (0.7 g) in tetrahydrofuran (20 ml), propionyl chloride (0.45 g) was added, and the resultant mixture was allowed to stand at room temperature overnight. The reaction mixture was concentrated, admixed with 5% hydrochloric acid and extracted with chloroform. The extract was concentrated to give an oily substance, which was purified by silica gel chromatography. Recrystallization from a mixture of toluene and hexane gave 1.17 g of N-methyl-2,4-dimethyl-5-(N-propionyl-N-trifluoromethanesulfonylamino)benzenesulfonamide (Compound No. 81). M.P., 101°-103° C.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. extractionextracted with chloroform
  3. concentrationThe extract was concentrated
  4. customto give an oily substance, which
  5. customwas purified by silica gel chromatography
  6. customRecrystallization
  7. additionfrom a mixture of toluene and hexane