反应详情

The product from step b, 3-acetylthiopropanoyl-L-proline-t-butyl ester, 0.5 g, was mixed with 4.5 ml of 5.5N methanolic ammonia at room temperature under nitrogen for one hour. The solvent was then removed at 25° C. with a rotary evaporator. After the product was taken up in methanol and reevaporated twice more in the rotary evaporator, the clear oily residue was dissolved in ethyl ether, washed twice with 5% potassium bisulphate and once with saturated NaCl, dried over MgSO4 and filtered. Residual solvent was removed in vacuo to yield a clear oily product, migrating as a single spot on thin layer chromatography in three separate solvent systems.

1. customThe solvent was then removed at 25° C. with a rotary evaporator
2. customreevaporated twice more in the rotary evaporator
3. dissolutionthe clear oily residue was dissolved in ethyl ether
4. washwashed twice with 5% potassium bisulphate and once with saturated NaCl
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customResidual solvent was removed in vacuo
8. customto yield a clear oily product
9. customseparate solvent systems