HRID1449505

反应详情

EQUATION

反应方程式

HRID 1449505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 100 ml of acetonitrile was dissolved 5.90 g of 4-aminothiophenol. To the solution were added 6.57 ml of triethylamine and 8.44 g of n-heptylbromide, followed by stirring at room temperature for 18 hours. The precipitated crystals were collected by filtration, followed by removing the solvent. To the residue was added water and the mixture was extracted with ethyl acetate. The extract was washed successively with 1N sodium hydroxide aqueous solution and saturated sodium chloride aqueous solution and dried over anhydrous potassium carbonate. After removing the solvent, the residue was purified by silica gel column chromatography using 50 g of silica gel and using chloroform as eluent to obtain 6.06 g of the titled compound.

WORKUP

后处理

  1. filtrationThe precipitated crystals were collected by filtration
  2. customby removing the solvent
  3. additionTo the residue was added water
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed successively with 1N sodium hydroxide aqueous solution and saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous potassium carbonate
  7. customAfter removing the solvent
  8. customthe residue was purified by silica gel column chromatography