1-碘-2-(甲氧基甲基)苯

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

实验步骤: A 10 mL oven-dried flask was charged with Mg turnings (88 mg, 3.6 mmol) andweactivated under vacuum by the use of a heat-gun. Under inert atmosphere was added a suspension of 1-Iodo-2-methoxymethylbenzene (0.67 g, 2.7 mmol) in Et2O (4 mL) and the reaction mixture was allowed to reflux for 1 hours. A suspension of compound 8 (0.38 g, 1.8 mmol) in CH2Cl2 (4 mL) was added via a syringe and the reaction mixture was stirred at rt overnight. The reaction mixture was quenched by addition of H2SO4 (10 mL, 2 M) and stirred at rt for 2 hours followed by addition of NaOH (10 mL, 2 M). Addition of THF (15 mL) was followed by extraction with ethyl acetate (3×50 mL) and the combined organic phases are washed with brine (10 mL) and NaOH (10 mL, 2 M), and the organic phases were dried (MgSO4) and evaporated to dryness to produce 0.51 g of crude 22. The crude product was subjected to CC [eluent:CH2Cl2:MeOH (99:1)] to give pure 22 (0.14 g, 23%); LC-MS [M+H]+ 331 (cald. 331.5). A 10 mL oven-dried flask Under inert atmosphere was added to reflux for 1 hours was added via a syringe The reaction mixture was quenched by addition of H2SO4 (10 mL, 2 M) stirred at rt for 2 hours followed by addition of NaOH (10 mL, 2 M) Addition of THF (15 mL) was followed by extraction with ethyl acetate (3×50 mL) the combined organic phases are washed with brine (10 mL) and NaOH (10 mL, 2 M) the organic phases were dried (MgSO4) evaporated to dryness to produce 0.51 g of crude 22