反应详情

温度

75 °C

Dissolve 2-bromo-5-fluoroaniline (25 g, 131 mmol) in methyldisulfide (220 mL) and heat to 75° C. under nitrogen. Add isoamyl nitrite (46 mL, 342 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 residue twice via silica gel chromatography eluting with hexanes to yield 22 g of 1-bromo-4-fluoro-2-methylsulfanyl-benzene (76%).

1. additionLarge exotherm may occur if addition
2. additionAfter addition
3. temperatureis complete heat
4. customthe reaction to 95° C. for 1 hour
5. temperaturecool to room temperature
6. concentrationconcentrate in vacuo
7. washPurify residue twice via silica gel chromatography eluting with hexanes