反应详情

A diastereomeric mixture of tert-butyl 2-methyl-1-oxo-4-phenyl-2,8-diazaspiro[4.6]undecane-8-carboxylate (step 4) (683.1 mg; 1.906 mmol) in DCM (6 ml) was treated with TFA (5.8 ml, 76 mmol) and stirred at RT for 10 minutes. The mixture was concentrated in vacuo and the crude product was dissolved in MeOH and applied to a 10 g pre-wetted (MeOH) SCX-2 cartridge. The column was washed with MeOH and the product was eluted with 2M NH3 in MeOH. The clean fractions were concentrated in vacuo to afford the title compound;

1. concentrationThe mixture was concentrated in vacuo
2. dissolutionthe crude product was dissolved in MeOH
3. washThe column was washed with MeOH
4. washthe product was eluted with 2M NH3 in MeOH
5. concentrationThe clean fractions were concentrated in vacuo