反应详情

A solution of 3-(3-methoxy-1-propoxy)-2-methyl-4-pyridone (0.32 g, 1.6 mmol) in 50 ml POCl3 was refluxed for 14 h. The POCl3 was evaporated off and the residue was partitioned between methylene chloride and water. The aqueous layer was separated, treated with K2CO3 until pH=10 and extracted with methylene chloride. The organic layer was dried over Na2SO4 and evaporated. The residue was purified by chromatography on silica gel with methanol/methylene chloride (3:97) as eluent. Evaporation off the solvent afforded 0.12 g (34%) product as a red oil.

1. customThe POCl3 was evaporated off
2. customthe residue was partitioned between methylene chloride and water
3. customThe aqueous layer was separated
4. additiontreated with K2CO3 until pH=10
5. extractionextracted with methylene chloride
6. dry with materialThe organic layer was dried over Na2SO4
7. customevaporated
8. customThe residue was purified by chromatography on silica gel with methanol/methylene chloride (3:97) as eluent
9. customEvaporation off the solvent