反应详情

1-[3-amino-6-(4-ethylsulfonylpiperazin-1-yl)pyrazin-2-yl]-2-bromo-ethanone (35 mg, 0.08922 mmol) was suspended in EtOH (2 mL) and 2 aminothiazole (8.935 mg, 0.08922 mmol) was added. The mixture was heated at reflux for 4 hours and then allowed to cool to ambient temperature. The solution was filtered through a 0.45 μnm PTFE filter and the solvent removed under a stream of nitrogen. The resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]. The fractions were collected and freeze-dried to give the title compound (55 mg, 10% Yield). 1H NMR (400.0 MHz, DMSO) d 1.14 (t, J=7.3 Hz, 3H), 3.01 (q, J=7.4 Hz, 2H), 3.21-3.23 (m, 4H), 3.34-3.36 (m, 4H), 7.28 (d, J=4.4 Hz, 1H), 7.67 (s, 1H), 7.89 (d, J=4.4 Hz, 1H) and 8.23 (s, 1H) ppm; MS (ES+) 394.0

1. temperatureThe mixture was heated
2. temperatureat reflux for 4 hours
3. filtrationThe solution was filtered through a 0.45 μnm PTFE
4. filtrationfilter
5. customthe solvent removed under a stream of nitrogen
6. customThe resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]
7. customThe fractions were collected
8. customfreeze-dried