HRID397274

反应详情

EQUATION

反应方程式

HRID 397274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous ammonia gas was passed into a solution of 4,4-dimethylpentane sulphonyl chloride (1.85 g) in dry tetrahydrofuran (5 ml) at 5-10° C. until saturation. The resulting suspension was stirred at room temperature for 18 hours and then evaporated under reduced pressure. The residue was partitioned between ethyl acetate (20 ml) and 2N aqueous hydrochloric acid (20 ml). The organic phase was separated, washed (brine 20 ml), dried (Na2SO4) and evaporated. Column chromatography on silica eluting with dichloromethane:methanol 98:2 gave 4,4-dimethylpentane sulphonic acid amide as an off-white solid (0.72 g).

WORKUP

后处理

  1. customevaporated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate (20 ml) and 2N aqueous hydrochloric acid (20 ml)
  3. customThe organic phase was separated
  4. washwashed (brine 20 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated