反应详情

In a 10 mL round bottomed flask was added a magnetic stirrer bar, 500 mg (1.2 mmol) of triphenylphosphonium methyl bromide and 137 mg (1.22 mmol) of potassium t-butoxide. The flask is stoppered with a rubber septum, flushed with nitrogen and 5 mL of dry THF was added to the mixture. After stirring at room temperature for 1 h, the solution was cooled to -60° C. and a solution of 170 mg (1.0 mmol) of 5-formyl4,6-dimethyl-2-aminopyridine in 2 mL of THF was added. After stirring for 30 minutes, the solution was warmed to 25° C. and stirred for 1 h. The solvent was removed in vacuo and and the title compound purified by silica gel column chromatography eluted with (methylene chloride/methanol (95:5).

1. additionIn a 10 mL round bottomed flask was added a magnetic stirrer bar
2. customflushed with nitrogen and 5 mL of dry THF
3. additionwas added to the mixture
4. temperaturethe solution was cooled to -60° C.
5. stirringAfter stirring for 30 minutes
6. temperaturethe solution was warmed to 25° C.
7. stirringstirred for 1 h
8. customThe solvent was removed in vacuo
9. customthe title compound purified by silica gel column chromatography
10. washeluted with (methylene chloride/methanol (95:5)