反应详情

温度

0 °C

To a cooled (0° C.) reaction mixture of [(4-methoxyphenyl)thio]acetaldehyde (36.4 mg, 0.2 mmol) and D-proline (4.6 mg, 0.04 mmol) in chloroform (1.2 mL) was added N-chlorosuccinimide. (26.7 mg, 0.2 mmol). The reaction mixture was stirred at 0° C. for 30 min, then gradually warmed to RT for 2 h. To the reaction mixture was added [6-(4-bromo-3-fluorophenyl)-1,2,4-triazin-3-amine (26.9 mg, 0.1 mmol). The reaction mixture was stirred for 1 h. The solvent was removed under reduced pressure. The residue was dissolved in isopropanol (2 mL) and heated at 100° C. overnight. After cooling, the reaction mixture was filtered and the filtrate was purified by RP-HPLC (pH=10) to afford the desired product. LCMS: (M+H)+=431.0.

1. temperatureTo a cooled
2. temperaturegradually warmed to RT for 2 h
3. stirringThe reaction mixture was stirred for 1 h
4. customThe solvent was removed under reduced pressure
5. dissolutionThe residue was dissolved in isopropanol (2 mL)
6. temperatureheated at 100° C. overnight
7. temperatureAfter cooling
8. filtrationthe reaction mixture was filtered
9. customthe filtrate was purified by RP-HPLC (pH=10)