反应详情

To a solution of tert-butyl {1-[2-(6-chloro-1-oxido-3-oxo-1,2,4-benzotriazin-4(3H)-yl)ethyl]piperidin-4-yl}carbamate (Intermediate 206) (0.43 g) in acetic acid (8 mL) and water (2 mL) was added zinc dust (0.50 g). After 30 minutes, the solution was filtered and the filtrate concentrated. The residue was then treated with potassium ferricyanide (1.0 g) in water (20mL). After 2 hours, the reaction was diluted with ethyl acetate. The aqueous layer was collected, the pH adjusted with solid Na2CO3 and extracted with ethyl acetate. The combined organic washes were dried (Na2SO4), filtered and concentrated. The residue was purified by chromatography on silica gel with 0-25% acetone in dichloromethane to yield 66 mg of the product.

1. filtrationthe solution was filtered
2. concentrationthe filtrate concentrated
3. additionThe residue was then treated with potassium ferricyanide (1.0 g) in water (20mL)
4. waitAfter 2 hours
5. additionthe reaction was diluted with ethyl acetate
6. customThe aqueous layer was collected
7. extractionextracted with ethyl acetate
8. dry with materialThe combined organic washes were dried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe residue was purified by chromatography on silica gel with 0-25% acetone in dichloromethane