反应详情

温度

90 °C

To an argon sparkled solution of XXIV (1 g, 3.04 mmol), and zinc cyanide (352 mg, 3 mmol) in DMF (5 mL) was added tetrakis-(triphenylphosphine) palladium (0) (300 mg, 0.228 mmol) and the reaction mixture was then heated at 90° C. overnight. When the mixture was cooled down and partitioned between EtOAc and water, the aqueous phase was separated and extracted with EtOAc. The combined organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated. The residue was purified by silica gel column to give (6-cyano-1,2,3,4-tetrahydro-quinolin-3-yl)-carbamic acid tert-butyl ester XXV (560 mg, 67%) as white solid.

1. temperatureWhen the mixture was cooled down
2. custompartitioned between EtOAc and water
3. customthe aqueous phase was separated
4. extractionextracted with EtOAc
5. washThe combined organic phase was washed with saturated NaCl
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. customThe residue was purified by silica gel column