反应详情

Analogously to Example 1, a solution of 0.629 g (1 mmol) of 1-[4-(pyridin-2-yl)-phenyl]-4(S)-hydroxy-2-amino-5(S)-N-(N-methoxycarbonyl-(L)-valyl)amino-6-phenyl-2-azahexane hydrochloride (Example 49 b) in 5 ml of DMF is added dropwise to a mixture of 0.303 g (1.6 mmol) of N-ethoxycarbonyl-(L)-valine, 0.575 g (3 mmol) of EDC, 0.27 g (2 mmol) of HOBT and 0.98 ml of TEA in 7 ml of DMF. After working up, the crude product is digested in DIPE and purified by subsequent medium-pressure column chromatography (SiO2 ; hexane/ethyl acetate) to yield the title compound. TLC: Rf =0.33 (ethyl acetate); HPLC20-100 : tRet =11.13. FAB MS (M+H)+ =691.

1. custompurified by subsequent medium-pressure column chromatography (SiO2 ; hexane/ethyl acetate)