反应详情

A solution of tert-butyl 1-((2R)-3-(benzyloxy)-1-(7-methyl-6-oxo-9-phenyl-2,7-diazaspiro[4.4]nonan-2-yl)-1-oxopropan-2-ylamino)-2-methyl-1-oxopropan-2-ylcarbamate (step 3) (206.5 mg) in DCM (4 mL) was treated with TFA (537 uL, 6.97 mmol). The reaction mixture was stirred at room temperature for 2 days. A further portion of TFA (2 ml) was added and stirring continued for 20 minutes. The mixture was concentrated in vacuo to afford a colourless oil. The oil was dissolved in MeOH and applied to a 10 g pre-wetted (MeOH) SCX-2 cartridge. The column was washed with MeOH (70 mL) and the product was eluted with 2M NH3 in MeOH (70 mL). The clean fractions were concentrated in vacuo to afford a colourless oil. The oil was further purified by mass-directed LC-MS to afford the title compound;

1. stirringstirring
2. waitcontinued for 20 minutes
3. concentrationThe mixture was concentrated in vacuo
4. customto afford a colourless oil
5. washThe column was washed with MeOH (70 mL)
6. washthe product was eluted with 2M NH3 in MeOH (70 mL)
7. concentrationThe clean fractions were concentrated in vacuo
8. customto afford a colourless oil
9. customThe oil was further purified by mass-directed LC-MS