反应详情

34 mg (0.11 mmol) cis-4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexylamine (13) were dissolved in 5 ml MeOH and 22 mg (0.22 mmol) triethylamine were added. After the reaction was stirred 30 min, 65 mg (1.1 mmol) acetic acid, 60 mg (0.22 mmol) 2-chloro-N-dimethylaminomethylene-5-formyl-benzenesulfonamide (73) and freshly dried molecular sieves were added and the mixture was stirred for 30 minutes at room temperature. A solution of 20.5 mg (0.33 mmol) sodium cyanoborohydride in 1 ml methanol was added and the mixture was allowed to stand at room temperature overnight. The solvent was removed i. vac. The residue was dissolved in dichloromethane, washed with 1N NaOH and brine, dried over MgSO4 and evaporated. 53 mg of the title compound were isolated as crude product and used without further purification. Rt=0.87 min (Method #4). Detected mass: 535.2/537.1 (M+H+).

1. stirringthe mixture was stirred for 30 minutes at room temperature
2. waitto stand at room temperature overnight
3. customThe solvent was removed i
4. dissolutionThe residue was dissolved in dichloromethane
5. washwashed with 1N NaOH and brine
6. dry with materialdried over MgSO4
7. customevaporated