反应详情

0.55 mL of benzoyl chloride was added to 10 mL of a methylene chloride solution containing 1.0 g of methyl 2-amino-4-bromobenzoate and 0.73 mL of triethylamine while ice-cooled and stirred at room temperature for 1 hour. The solvent was evaporated under reduced pressure and a saturated sodium hydrogen carbonate aqueous solution and ethyl acetate were added to the residue. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with 1.0 mol/L hydrochloric acid and a saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the obtained residue and a solid substance was separated by filtration to obtain 0.9 g of methyl 2-(benzamido)-4-bromobenzoate as while solid.

1. temperaturecooled
2. customThe solvent was evaporated under reduced pressure
3. additiona saturated sodium hydrogen carbonate aqueous solution and ethyl acetate were added to the residue
4. customThe organic layer was separated
5. dry with materialdried over anhydrous magnesium sulfate
6. washafter washed with 1.0 mol/L hydrochloric acid
7. customa saturated sodium chloride aqueous solution sequentially, and the solvent was evaporated under reduced pressure
8. additionDiisopropyl ether was added to the obtained residue
9. customa solid substance was separated by filtration