反应详情

温度

0 °C

3-(6-Methoxy-7-oxiranylmethoxy-quinolin-4-yloxy)-5,6,5′-trimethyl-[2,2′]bipyridine (compound 457) (54 mg) was dissolved in methylene chloride (2 ml) to prepare a solution which was then brought to 0° C. Trifluoroacetic acid (1 ml) was added thereto, and the mixture was stirred at 0° C. for 30 min and then at room temperature for 5 hr. The reaction solution was brought to 0° C., was stirred and was made alkaline by the addition of a 10% aqueous sodium hydroxide solution. Water was added to the reaction solution, the mixture was extracted with chloroform, and the chloroform layer was then washed with saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (35 mg, yield 63%).

1. customto prepare a solution which
2. customwas then brought to 0° C
3. waitat room temperature for 5 hr
4. customwas brought to 0° C.
5. stirringwas stirred
6. extractionthe mixture was extracted with chloroform
7. washthe chloroform layer was then washed with saturated brine
8. dry with materialwas dried over anhydrous sodium sulfate
9. customThe solvent was removed by distillation under the reduced pressure
10. customthe residue was purified by thin layer chromatography