反应详情

To a stirred solution of 6-(1-aminoethyl)-N-[4-(methyloxy)phenyl]-1,2,4-triazin-3-amine (Intermediate 47) (100 mg, 0.41 mmol), 5-bromothiophene-2-carboxylic acid (93 mg, 0.45 mmol) and O-(7-azabenzotriazol-1-yl-N,N,N′N′-tetramethyluronium hexafluorophospahte (186 mg, 0.49 mmol) in N,N-dimethylformamide (5 mL) was added triethylamine (0.170 mL, 1.22 mmol) and the resulting mixture stirred at room temperature, under nitrogen, for 2 h 50 min. The mixture was then reduced under vacuum and the residue purified by SPE (Si, 10 g cartridge) eluting with hexane/ethyl acetate (10:1 to 0:1) and then methanol. The appropriate fractions containing product were combined and then purified further by SPE (SCX, 5 g cartridge) eluting with methanol then ammonia in methanol (0.5 N to 2.0 N) to afford 5-bromo-N-[1-(3-{[4-(methyloxy)phenyl]amino}-1,2,4-triazin-6-yl)ethyl]-2-thiophenecarboxamide (109 mg) as a yellow solid. MS m/z 434/436 (M+1).

1. customthe residue purified by SPE (Si, 10 g cartridge)
2. washeluting with hexane/ethyl acetate (10:1 to 0:1)
3. additionThe appropriate fractions containing product
4. custompurified further by SPE (SCX, 5 g cartridge)
5. washeluting with methanol