反应详情

To a solution of 2,4-difluoro-1-methylbenzene (6 g, 47 mmol) in trifluoroacetic acid (15 mL) was added N-iodosuccinimide (12.1 g). The mixture was stirred at rt overnight before it was poured into ice and extracted with hexanes. The organic layer was separated and washed with saturated Na2S2O3, NaHCO3, brine and then dried over MgSO4. The crude product was purified by silica gel chromatography to give 94A (10.7 g, 90% yield) as a colorless oil. 1H NMR (400 MHz, CDCl3) δ ppm 2.15-2.30 (m, 3H) 6.73-6.85 (m, 1H) 7.55 (t, J=7.69 Hz, 3H).

1. additionwas poured into ice
2. extractionextracted with hexanes
3. customThe organic layer was separated
4. washwashed with saturated Na2S2O3, NaHCO3, brine
5. dry with materialdried over MgSO4
6. customThe crude product was purified by silica gel chromatography