反应详情

温度

50 °C

153 mg (0.315 mmol) trans-N-[4-(5-bromo-pentyl)-cyclohexylmethyl]-N-methyl-4-trifluoromethyl-benzenesulfonamide (example 1.6) dissolved in 2.0 ml of methanol were treated with 0.5 ml of N-allyl-methyl-amine and the reaction mixture stirred for 6 h at 50° C. It was then evaporated, poured into 50 ml of an ice/water mixture and extracted 3 times with 50 ml of dichloromethane. The combined dichloromethane phases were washed with sodium carbonate solution, dried over magnesium sulfate and evaporated under reduced pressure. The residue formed was chromatographed on silica gel with a 9:1:0.1 v/v/v mixture of dichloromethane, methanol and saturated ammonia solution as the eluent giving 0.110 g (73.3%) trans-N-{4-[5-(allyl-methyl-amino)-pentyl]-cyclohexylmethyl}-N-methyl-4-trifluoromethyl-benzenesulfonamide as colorless solid, MS: 475 (MH+).

1. customIt was then evaporated
2. additionpoured into 50 ml of an ice/water mixture
3. extractionextracted 3 times with 50 ml of dichloromethane
4. washThe combined dichloromethane phases were washed with sodium carbonate solution
5. dry with materialdried over magnesium sulfate
6. customevaporated under reduced pressure
7. customThe residue formed
8. customwas chromatographed on silica gel with a 9:1:0.1 v/v/v mixture of dichloromethane, methanol and saturated ammonia solution as the eluent