反应详情

To a solution of 18 (47.8 mg, 0.144 mmol), copper(II) chloride (80 mg) and dimethylamine (100 μl) in DMF (16 mL) was bubbled in oxygen for 7 h. The reaction mixture was concentrated in vacuum to about 5 mL, and was then diluted with water. A solution of saturated ammonium chloride was used to adjusted the pH of the above mixture to about 6, and the resulting mixture was extracted with chloroform (10 mL×10). The combined extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was flash chromatographed with 2% methanol in chloroform to give dl-camptothecin (45.5 mg, 91%).

1. concentrationThe reaction mixture was concentrated in vacuum to about 5 mL
2. additionwas then diluted with water
3. extractionthe resulting mixture was extracted with chloroform (10 mL×10)
4. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customchromatographed with 2% methanol in chloroform