反应详情

A DMF solution (10 mL) containing 31-3 (301 mg, 1.0 mmol) 2-1 (336 mg, 1.0 mmol), HOBT (206 mg, 1.35 mmol), EDC (258 mg, 1.35 mmol) and NMM (440 μl, 4.0 mmol) was stirred under ambient conditions for 18 h. The DMF was evaporated and the residue partitioned between CH2Cl2 and H2O. The organic layer was dried (MgSO4) and concentrated to a yellow gum which was purified by flash chromatography (silica, 4:1, CHCl3 ·NH3 /IPA) to provide impure 31-4 which was rechromatographed (silica, 9:1 EtOAc/IPA) to give 31-4 as a colorless foam.

1. customThe DMF was evaporated
2. customthe residue partitioned between CH2Cl2 and H2O
3. dry with materialThe organic layer was dried (MgSO4)
4. concentrationconcentrated to a yellow gum which
5. customwas purified by flash chromatography (silica, 4:1, CHCl3 ·NH3 /IPA)
6. customto provide impure 31-4 which
7. customwas rechromatographed (silica, 9:1 EtOAc/IPA)