反应详情

To tert-butyl 1-((2R)-1-(4-(4-fluorophenyl)-2-methyl-1-oxo-2,7-diazaspiro[4.5]decan-7-yl)-3-(4-methylbenzyloxy)-1-oxopropan-2-ylamino)-2-methyl-1-oxopropan-2-yl(methyl)carbamate (128 mg, 0.196 mmol) in DCM (2 ml) was added TFA (0.6 ml, 7.79 mmol). The mixture was stirred at RT for 30 mins then concentrated in vacuo. The residue was suspended in sat. sodium bicarbonate soln. (10 ml) and extracted with EtOAc (2×50 ml). The extracts were dried and concentrated. The residue was applied to a 20 g silica cartridge in DCM and this was eluted with 5% MeOH/DCM [diluted from 10% MeOH/DCM containing 1% aqueous 880 ammonia]. The relevant fractions were combined and concentrated to give a foam. This was dried at 40° C. overnight under vacuum to give the title compound as a glass.

1. concentrationthen concentrated in vacuo
2. extraction(10 ml) and extracted with EtOAc (2×50 ml)
3. customThe extracts were dried
4. concentrationconcentrated
5. washthis was eluted with 5% MeOH/DCM [diluted from 10% MeOH/DCM containing 1% aqueous 880 ammonia]
6. concentrationconcentrated
7. customto give a foam
8. customThis was dried at 40° C. overnight under vacuum