反应详情

温度

40 °C

To a solution of DMF (18.04 mmoles) in DCM (10 ml) there is added POCl3, dropwise, at 0° C. After stirring for 5 minutes, a solution of the compound obtained in Step A (9.02 mmoles) is added dropwise. After stirring for 3 hours at 0° C., the reaction mixture is heated at 40° C. for 30 minutes. At ambient temperature, an aqueous solution of potassium acetate (32 mmoles) is added and then the reaction mixture is stirred at 40° C. for 30 minutes. At ambient temperature, the solution is brought to alkaline pH using 2M NaOH solution and is then extracted with DCM. The organic phase is washed with water and with saturated NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The residue obtained is purified on silica gel (SiO2; gradient DCM/AcOEt) to yield the title product.

1. customat 0° C
2. stirringAfter stirring for 3 hours at 0° C.
3. stirringthe reaction mixture is stirred at 40° C. for 30 minutes
4. customAt ambient temperature
5. extractionis then extracted with DCM
6. washThe organic phase is washed with water and with saturated NaCl solution
7. dry with materialdried over sodium sulphate
8. filtrationfiltered
9. customevaporated to dryness
10. customThe residue obtained
11. customis purified on silica gel (SiO2; gradient DCM/AcOEt)