反应详情

温度

75 °C

Dissolve 2-bromo-4,6-difluoroaniline (40 g, 192 mmol) in methyldisulfide (250 mL) and heat to 75° C. under nitrogen. Add isoamyl nitrite (67 mL, 500 mmol) dropwise via an addition funnel trough a reflux condenser (˜1 drop/sec). Large exotherm may occur if addition is too fast. After addition is complete, heat the reaction to 95° C. for 1 hour and cool to room temperature and concentrate in vacuo. Purify dark brown residue via silica gel chromatography eluting with hexanes to yield 30.3 g of 1-bromo-3,5-difluoro-2-methylsulfanyl-benzene (66%).

1. additionLarge exotherm may occur if addition
2. additionAfter addition
3. temperatureheat
4. customthe reaction to 95° C. for 1 hour
5. temperaturecool to room temperature
6. concentrationconcentrate in vacuo
7. customPurify dark brown residue via silica gel chromatography
8. washeluting with hexanes