HRID2057245

反应详情

EQUATION

反应方程式

HRID 2057245 的结构方程式

PROCEDURE

实验过程

A solution of 69 mg (0.146 mmol) of trans-N-[4-(3-Bromo-propoxymethyl)-cyclohexyl]-N-methyl-4-trifluoromethyl-benzenesulfonamide in 0.8 ml DMA was treated at 0° C. with 0.028 ml (0.29 mmol) of N-allylmethylamine and stirred at RT for 22 h. The solution was cooled (0° C.) and treated again with 0.028 ml (0.29 mmol) of N-allylmethylamine. After 6 h at RT, the solution was concentrated and dissolved in aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried over Na2SO4 and evaporated. Flash column chromatography on silica gel with CH2Cl2/MeOH (95:5) yielded 43 mg (64%) of trans-N-{4-[3-(Allyl-methyl-amino)-propoxymethyl]-cyclohexyl}-N-methyl-4-trifluoromethyl-benzenesulfonamide, MS: 463 (MH+).

WORKUP

后处理

  1. temperatureThe solution was cooled (0° C.)
  2. waitAfter 6 h at RT
  3. concentrationthe solution was concentrated
  4. dissolutiondissolved in aqueous saturated NaHCO3/Et2O (3×)
  5. dry with materialThe organic phase was dried over Na2SO4
  6. customevaporated