HRID1805308

反应详情

EQUATION

反应方程式

HRID 1805308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 7.07 g (20 mmol) of methyltriphenylphosphonium bromide in 50 mL of dry THF at 0° C. were added t-BuLi of (14.7 ml, 1.5 M in hexane) and the solution turned brown. After 1 hour of stirring at 0° C., the crude 1-(4-Iodo-phenyl)-2-methyl-propan-1-one from the last step in 20 mL of THF were added dropwise and the solution was stirred for 14 hours at room temperature. After cooling to ca. 20° C., 52 mL of water were added and the solution was extracted with dichloromethane (3×50 mL). The organic layer was dried over MgSO4 and the solvent was removed to give the crude title compound as white solid. The product was used for the next step without further purification.

WORKUP

后处理

  1. stirringthe solution was stirred for 14 hours at room temperature
  2. temperatureAfter cooling to ca. 20° C.
  3. extractionthe solution was extracted with dichloromethane (3×50 mL)
  4. dry with materialThe organic layer was dried over MgSO4
  5. customthe solvent was removed