反应详情

温度

0 °C

2-(3-methoxy-phenyl)-2-methyl-propionic acid (24.40 g) is dissolved in toluene (120 mL) and cooled to 0° C. Triethylamine (16.61 mL) and diphenylphosphorylazide (24.37 g) are added. After 0.5 h the mixture is heated to 110° C. After 3 h the reaction mixture is diluted with EtOAc, cooled to 0° C., extracted with NaHCO3 solution and NaCl solution (H2O, 10%), dried on magnesium sulphate, filtered off from the desiccant and the solvent is eliminated in vacuo. The residue is used in the next reaction step without any further purification.

1. temperatureAfter 0.5 h the mixture is heated to 110° C
2. temperaturecooled to 0° C.
3. extractionextracted with NaHCO3 solution and NaCl solution (H2O, 10%)
4. customdried on magnesium sulphate
5. filtrationfiltered off from the desiccant and the solvent
6. customThe residue is used in the next reaction step without any further purification