反应详情

N-(tert-Butoxycarbonyl)-4-iodo-(L)-phenylalaninamide (4.24 g) was dissolved in DCM (20 mL) and to the solution was added TFA (20 mL). The reaction mixture was stirred, at room temperature, for 0.5 h then concentrated to dryness under reduced pressure. The crude material obtained was loaded onto an SCX cartridge. Non-basic impurities were washed off with a 1:1 mixture of DCM and methanol, then the cartridge was eluted with 10% ammonia in methanol. Eluent from the latter was concentrated to dryness to give the free base of the sub-title compound (3 g) as a white solid.

1. concentrationthen concentrated to dryness under reduced pressure
2. customThe crude material obtained
3. washNon-basic impurities were washed off with a 1:1 mixture of DCM and methanol
4. washthe cartridge was eluted with 10% ammonia in methanol
5. concentrationEluent from the latter was concentrated to dryness