反应详情

A solution of 103 (2.25 mmol) and NaN3 (731 mg, 11.25 mmol) in DMF (15 ml) is heated at 70° C. in a sealed tube overnight. The solvent is removed in vacuo and water (10 ml) and EtOAc (10 ml) are added to the residue. The layers are separated and the aqueous layer is extracted with EtOAc (2×10 ml). The combined extracts are washed with brine (15 ml) and dried with Na2SO4. The solvent is removed in vacuo and the resulting yellow oil (104) is used in the next step without further purification.

1. customThe solvent is removed in vacuo and water (10 ml) and EtOAc (10 ml)
2. additionare added to the residue
3. customThe layers are separated
4. extractionthe aqueous layer is extracted with EtOAc (2×10 ml)
5. washThe combined extracts are washed with brine (15 ml)
6. dry with materialdried with Na2SO4
7. customThe solvent is removed in vacuo
8. customthe resulting yellow oil (104) is used in the next step without further purification