反应详情

温度

85 °C

A mixture of 121 (10 mmol) and POCl3 (25 ml) is heated at 85° C. for 4 hours. The solvent is removed in vacuo and EtOAc (40 ml) and water (30 ml) are added to the residue. NaHCO3 is carefully added until the pH of the aqueous layer is greater than 7. The layers are separated and the aqueous layer is extracted with EtOAc (2×30 ml). The combined extracts are washed with brine (50 ml), dried (Na2SO4) and evaporated. Flash column purification of the residue with 3:1 EtOAc, hexane provides the product (122) as a light yellow oil.

1. customThe solvent is removed in vacuo and EtOAc (40 ml) and water (30 ml)
2. additionare added to the residue
3. additionNaHCO3 is carefully added until the pH of the aqueous layer
4. customThe layers are separated
5. extractionthe aqueous layer is extracted with EtOAc (2×30 ml)
6. washThe combined extracts are washed with brine (50 ml)
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customFlash column purification of the residue with 3:1 EtOAc, hexane