反应详情

温度

20 °C

To a solution of compound 49 ((4-chloro-benzyl)-{1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carbonyl}-amino)-acetic acid (1 eq.) in DMF was added EDC.HCl (1.3 eq.), DMAP (1.3 eq.) and trifluoromethanesulfonamide (1.3 eq.). The reaction was stirred for 15 h at 20° C. The crude was concentrated under reduced pressure then partitioned between water and EtOAc. The layers were separated and the organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by preparative LCMS to afford 1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carboxylic acid (4-chloro-benzyl)-(2-oxo-2-trifluoromethanesulfonylamino-ethyl)-amide.

1. concentrationThe crude was concentrated under reduced pressure
2. customthen partitioned between water and EtOAc
3. customThe layers were separated
4. dry with materialthe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude was purified by preparative LCMS