反应详情

温度

-70 °C

A solution of methyl 2-(4'-trimethylsilyloxyphenyl)ethanoate (34.3 mmole) in dimethoxyethane (10 ml) was added dropwise to the reaction, the temperature rising to -30° C. before cooling to -70° C. This cold reaction mix was added dropwise to a solution of methyliodide (0.16 mole) in dimethoxyethane (20 ml) cooled to -70° C. The mixture was stirred at room temperature overnight before removing the solvent by evaporation. The residue was stirred with dilute HCl and extracted with dichloromethane, washed with saturated NaHCO3 solution, dried (MgSO4) and the product isolated by evaporation. Distillation of the crude product gave MHPP (yield 88%).

1. customrising to -30° C.
2. customThis cold reaction
3. additionmix
4. temperaturecooled to -70° C
5. custombefore removing the solvent
6. customby evaporation
7. stirringThe residue was stirred with dilute HCl
8. extractionextracted with dichloromethane
9. washwashed with saturated NaHCO3 solution
10. dry with materialdried (MgSO4)
11. customthe product isolated by evaporation
12. distillationDistillation of the crude product