反应详情

To the crude 3-tert-butoxycarbonyl-6-(4-bromomethyl-benzylthio)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine in anhydrous DMF (1 mL) under nitrogen, add with string sodium methanesulfinate (400 mg, 3.9 mmol), and continue stirring for 30 min at ambient temperature followed by 2 h at 40° C. Add water, extract three times with EtOAc, wash with brine, dry over anhydrous MgSO4, and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (3:1) to give a clear oil that solidifies on standing to a white solid (118 mg, 61%).

1. waitfollowed by 2 h at 40° C
2. extractionAdd water, extract three times with EtOAc
3. washwash with brine
4. dry with materialdry over anhydrous MgSO4
5. concentrationconcentrate in vacuo
6. customPurify by chromatography on silica gel eluting with hexane/EtOAc (3:1)
7. customto give a clear oil