反应详情

To the product of Example 21 (6.7 g, 42.9 mmol) in 300 mL of acetonitrile (CH3CN), was added potassium cyanide (KCN, 11.2 g, 171.7 mmol) and dibenzo-18-crown-6 (1.0 g, 2.8 mmol). After the reaction had been refluxed for 18 hours, it was cooled to room temperature, and stripped of all solvent under reduced pressure. The residue was partitioned between 100 mL each of water and CH2Cl2 and the aqueous phase was washed with 3×100 mL of CH2Cl2. The combined organic phase was dried (Na2SO4), filtered, and stripped of solvent to yield 6.7 g of crude product. This material was purified by HPLC on silica gel to yield 5.3 g of the title material as a yellow oil.

1. temperatureAfter the reaction had been refluxed for 18 hours
2. customThe residue was partitioned between 100 mL each of water and CH2Cl2
3. washthe aqueous phase was washed with 3×100 mL of CH2Cl2
4. dry with materialThe combined organic phase was dried (Na2SO4)
5. filtrationfiltered
6. customto yield 6.7 g of crude product
7. customThis material was purified by HPLC on silica gel