HRID2119817

反应详情

EQUATION

反应方程式

HRID 2119817 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(2-amino-2-methylpropyl)aniline hydrochloride salt (1.0 g, 4.98 mmol) in anhydrous DMF (30 mL) was treated with benzenesulfonyl chloride (880 mg, 4.98 mmol). The solution was stirred at ambient temperature for 16 h. The solvent was removed under reduced pressure and the residue was washed twice with hexane. The insoluble material was dissolved in water and extracted twice with ethyl ether to remove any remaining neutral impurities. The aqueous layer was separated and basified with excess 1N sodium hydroxide. Upon standing, a crystalline solid soon precipitated. The solid was collected, and dried under vacuum at 60° C. to provide 570 mg (38%) of the desired product as a white crystalline solid. Mp 180-181° C.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. washthe residue was washed twice with hexane
  3. dissolutionThe insoluble material was dissolved in water
  4. extractionextracted twice with ethyl ether
  5. customto remove any remaining neutral impurities
  6. customThe aqueous layer was separated
  7. customa crystalline solid soon precipitated
  8. customThe solid was collected
  9. customdried under vacuum at 60° C.