反应详情

A mixture of (8-methoxyquinolin-2-yl)methanol (1.0 g, 5.3 mmol) and N,N-dimethylformamide (39 mg, 0.53 mmol) in sulfurous dichloride (20 mL) was stirred at room temperature for 2 h. The reaction mixture was concentrated and ice water was added. The pH of the aqueous layer was adjusted to 7 with 10 N sodium hydroxide solution. The mixture was extracted with DCM (30 mL×3). The combined organic phase was dried with anhydrous sodium sulfate, concentrated, and purified by column chromatography to give 0.66 g of the product as a yellow solid. MS (ESI): m/z 208.0 [M+H]+.

1. concentrationThe reaction mixture was concentrated
2. additionice water was added
3. extractionThe mixture was extracted with DCM (30 mL×3)
4. dry with materialThe combined organic phase was dried with anhydrous sodium sulfate
5. concentrationconcentrated
6. custompurified by column chromatography