反应详情

Ethyl 3-((R)—((R)-1,1-dimethylethylsulfinamido)(phenyl)methyl)phenyl(methyl)phosphinate, 24-d, (15 g, 80% purity, 32.3 mmol) was dissolved in HCl/dioxane (70 ml, 4 mol/L) and the mixture was stirred at room temperature for 2 h. The mixture was concentrated under vacuum and the residue was dissolved with H2O (90 ml) and HCl (10 ml). The aqueous phase was extracted with EA (80 ml*5). The pH of the aqueous layer was adjusted to about pH=12 and extracted with EA (100 ml*3). The organic was dried over Na2SO4 and the crude product was purified with column (DCM/MeOH=100/1˜30/1) to provide the product, 24-e, (6.77 g, 74%).

1. concentrationThe mixture was concentrated under vacuum
2. dissolutionthe residue was dissolved with H2O (90 ml) and HCl (10 ml)
3. extractionThe aqueous phase was extracted with EA (80 ml*5)
4. extractionextracted with EA (100 ml*3)
5. dry with materialThe organic was dried over Na2SO4
6. customthe crude product was purified with column (DCM/MeOH=100/1˜30/1)