反应详情

To 4 mL of a dichloromethane solution containing 0.07 mL of oxalyl chloride, 0.11 mL of dimethylsulfoxide was added dropwise under nitrogen atmosphere at −60° C., and stirred for 10 min. 10 mL of a dichloromethane solution containing 0.14 g of 1-(2-hydroxyethyl)-8-methoxyquinolin-2(1H)-one was added dropwise at the same temperature, and stirred for 12 min. After 0.36 mL of triethylamine was added at the same temperature, it was stirred at room temperature for 1.5 hours, and 20 mL of water was added. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and extracts were combined, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to give (8-methoxy-2-oxoquinolin-1(2H)-yl)acetaldehyde as a pale yellow solid.

1. additionwas added dropwise under nitrogen atmosphere at −60° C.
2. additionwas added dropwise at the same temperature
3. stirringstirred for 12 min
4. stirringwas stirred at room temperature for 1.5 hours
5. customThe organic layer was separated
6. extractionthe aqueous layer was extracted with chloroform
7. dry with materialdried over anhydrous magnesium sulfate
8. customthe solvent was removed under reduced pressure