反应详情

To a solution of (2-chloro-5-(Boc-amino)phenyl)acetonitrile (5.2 g; 20 mmol; from step (iii) above) in water:i-PrOH (37 mL; 2:1) was added KOH (5 g; 89 mmol), and the solution was refluxed overnight. The mixture was subsequently concentrated, water:THF (50 mL; 1:1) and Boc2O were added, and the mixture was stirred overnight. The THF was evaporated, the water phase was washed with ether (1×50 mL), made acidic with HCl (dilute) and extracted with EtOAc (3×30 mL). The combined organic layers were washed with water, dried (Na2SO4) and concentrated, yielding 2.8 g (50%) of the sub-title compound.

1. temperaturethe solution was refluxed overnight
2. concentrationThe mixture was subsequently concentrated
3. additionwater:THF (50 mL; 1:1) and Boc2O were added
4. customThe THF was evaporated
5. washthe water phase was washed with ether (1×50 mL)
6. extractionextracted with EtOAc (3×30 mL)
7. washThe combined organic layers were washed with water
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated