反应详情

Analogously to Example 1, a solution of 1.26 g (2 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 49b) in 12 ml of DMF is added dropwise to a mixture of 0.6 g (3.2 mmol) of N-methoxycarbonyl-(L)-iso-leucine, 1.14 g (6 mmol) of EDC, 0.54 g (4 mmol) of HOBT and 1.68 ml of TEA in 13 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 =0.32 (ethyl acetate); HPLC20-100 : tRet =11.04. FAB MS (M+H)+ =691.

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