反应详情

温度

65 °C

Few crystals of iodine are added to tetrahydrofuran (200 mL) containing magnesium turnings (2.8 g, 0.117 mol). The mixture is heated at 60-70° C. A solution of 4-bromo-2-chlorobiphenyl (26 g, 0.097 mol) in tetrahydrofuran (50 mL) is added dropwise to the reaction mixture and refluxed for 1 hr. Reaction mixture is brought to room temperature and then cooled to −20° C. Carbon dioxide gas is passed through the reaction mixture for 45 minutes. The reaction mixture is treated with 3N HCl (125 mL) and extracted with ethyl acetate (2×200 mL). Combined organic layer is dried over sodium sulphate. Removal of solvent under reduced pressure gives a solid which is washed with diethyl ether (2×100 mL) and then dried to furnish 2-chlorobiphenyl-4-carboxylic acid.

1. temperaturerefluxed for 1 hr
2. customReaction mixture
3. customis brought to room temperature
4. temperaturecooled to −20° C
5. extractionextracted with ethyl acetate (2×200 mL)
6. dry with materialCombined organic layer is dried over sodium sulphate
7. customRemoval of solvent under reduced pressure
8. customgives a solid which
9. washis washed with diethyl ether (2×100 mL)
10. customdried