反应详情

4-[6-(4-Cyano-phenyl)-2-oxo-3,3-bis-(1-trityl-1H-imidazol-4-ylmethyl)-2,3-dihydro-indol-1-ylmethyl]-N,N-dimethyl-benzenesulfonamide (0.3 g, 0.4 mmol) was dissolved in a solution of 4.0 ml of TFA and 500 μL of triethylsilane under an atmosphere of dry N2 and stirred for 1 hour. The heterogeneous mixture was concentrated under vacuum and partitioned between aqueous 0.1 N HCl and ethyl ether (Et2O). The water layer was washed with Et2O and then basified to pH˜9 with sodium hydroxide (NaOH). The water layer was then washed 3 times with DCM. The DCM layers were combined and dried over Na2SO4, filtered and concentrated under vacuum to give 13 mg of the titled compound as a purple solid.

1. concentrationThe heterogeneous mixture was concentrated under vacuum
2. custompartitioned between aqueous 0.1 N HCl and ethyl ether (Et2O)
3. washThe water layer was washed with Et2O
4. washThe water layer was then washed 3 times with DCM
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum