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