反应详情

温度

25 °C

A dry, argon-filled Schlenk tube with a magnetic stirrer bar and septum is initially charged with 2,4-difluoro-1-nitrobenzene (159 mg, 1 mmol) in anhydrous THF (2 ml). After adding (TMP)2Zn.MgCl2 (3.00 ml, 1.2 mmol) at 25° C., the mixture is stirred for 30 min, then a solution of iodine (381 mg, 1.5 mmol) in anhydrous THF (2 ml) is added dropwise and the mixture is stirred at 25° C. overnight. For workup, the mixture is diluted with aqueous sat. NH4Cl solution (30 ml) and aqueous sat. Na2S2O3 solution (30 ml) and extracted with ethyl acetate (3×30 ml). After the combined organic phases have been dried over Na2SO4, the solvent has been distilled off and purification has been effected by column chromatography on silica gel (heptane:ethyl acetate), the desired compound (210 mg, 74% of theory) was obtained as a colourless crystalline product.

1. additionA dry, argon-filled Schlenk tube with a magnetic stirrer bar
2. additionAfter adding (TMP)2Zn
3. extractionextracted with ethyl acetate (3×30 ml)
4. dry with materialAfter the combined organic phases have been dried over Na2SO4
5. distillationthe solvent has been distilled off
6. custompurification