Iodine chloride → 4-Bromo-2-iodo-5-(trifluoromethyl)aniline

温度

60 °C

4-Bromo-3-trifluoromethyl-phenylamine (1.00 g, 4.17 mmol) was dissolved in acetic acid (5 ml). Iodine monochloride (1 M solution in dichloromethane, 5 ml) was added and the mixture was stirred at 60° C. overnight. The reaction solution was poured into a mixture of ice and a saturated aqueous sodium bicarbonate solution and then extracted with ethyl acetate. The organic layer was washed with an aqueous sodium bicarbonate solution, an aqueous sodium thiosulfate solution, water and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane-ethyl acetate) to give 4-bromo-2-iodo-5-trifluoromethyl-phenylamine (889 mg, 58%).

1. additionThe reaction solution was poured into a mixture of ice
2. extractiona saturated aqueous sodium bicarbonate solution and then extracted with ethyl acetate
3. washThe organic layer was washed with an aqueous sodium bicarbonate solution
4. dry with materialan aqueous sodium thiosulfate solution, water and saturated brine, dried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (n-hexane-ethyl acetate)

ORDレコード

ord-84d1200c253043868538eea4ffee1607

出典データセット

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09169254B2