1-(4-碘苯基)-2-甲基丙-1-one

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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. the solution was stirred for 14 hours at room temperature After cooling to ca. 20° C. the solution was extracted with dichloromethane (3×50 mL) The organic layer was dried over MgSO4 the solvent was removed

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 2.0 M solution of Isopropylmagnesium chloride (10 ml, 20 mmol) was added dropwise (30 min), under nitrogen, to a stirred solution of freshly distilled 4-iodobenzoyl chloride (5.32 g, 20 mmol) and Fe(acac)3 (0.35 g, 1 mmol) in 150 ml of dry THF at room temperature. After addition, the stirring was continued for 10 min at the same temperature. The reaction was quenched by pouring the mixture into dilute hydrochloric acid and extracted with several portions of ether. The combined ether extracts were washed with aq. NaHCO3, water, and dried over Na2SO4. Removal of the organic solvents under vacuum gave the product as colorless oil. And the crude product was used for the next step without further purification. at room temperature After addition The reaction was quenched by pouring the mixture into dilute hydrochloric acid extracted with several portions of ether The combined ether extracts were washed with aq. NaHCO3, water dried over Na2SO4 Removal of the organic solvents under vacuum