反应详情

Di-tert-butyl 2-(4-((R)-3-(4-(N-(4-(4-((R)-(tert-butyldimethylsilyloxy)(4′-chlorobiphenyl-2-yl)methyl)piperidin-1-yl)benzoyl)sulfamoyl)-2-(trifluoromethylsulfonyl)phenylamino)-4-(phenylthio)butyl)piperazin-1-yl)ethyl phosphate (INTERMEDIATE 62,414 mg, 0.32 mmol) was dissolved in DCM (0.5 ml) and treated with a solution of HCl (4M in dioxane, 4.0 ml, 15.84 mmol) at rt, to provide a cloudy solution. The reaction mixture was concentrated under reduced pressure to provide an oily residue which was purified by reverse phase HPLC (Gilson column, eluting with 20→95% MeCN in 10 mM NH4OAc with 5% MeCN over 15 min). The collected fractions were concentrated and washed with water and filtered to remove NH4OAc and provide the title compound (120 mg, yield: 35%).

1. customto provide a cloudy solution
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. customto provide an oily residue which
4. customwas purified by reverse phase HPLC (Gilson column, eluting with 20→95% MeCN in 10 mM NH4OAc with 5% MeCN over 15 min)
5. concentrationThe collected fractions were concentrated
6. washwashed with water
7. filtrationfiltered
8. customto remove NH4OAc