反应详情

A mixture of 3 (10.35 g, 60.1 mmol), imidazole (8.18 g, 120.2 mmol), and TBDPSCl (15.6 ml, 60.1 mmol) in DMF (40 ml) was stirred for 16 h at room temperature under positive pressure of dry Ar. The mixture was partitioned between EtOAc and sat. aqueous NaHCO3. The organic layer was dried (Na2SO4) and evaporated. The resulting syrupy residue was treated with MeOH (ca. 40 ml) to give the precipitated 4. This procedure was repeated further 3 times to give 4 (18.97 g, 77%) as a white solid.

1. customThe mixture was partitioned between EtOAc and sat. aqueous NaHCO3
2. dry with materialThe organic layer was dried (Na2SO4)
3. customevaporated
4. additionThe resulting syrupy residue was treated with MeOH (ca. 40 ml)
5. customto give the
6. customprecipitated 4