反应详情

0.52 mL of triethylamine and 0.16 mL of benzoyl chloride were added to 3.8 mL of methylene chloride suspension containing 0.39 g of methyl 2-amino-4-((phenylthio)methyl)benzoate hydrochloride while ice-cooled and stirred at room temperature for 3 hours and 30 minutes. The solvent was evaporated under reduced pressure and ethyl acetate and 1.0 mol/L hydrochloric acid were added to the obtained residue. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with a saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution sequentially, and the solvent vas evaporated under reduced pressure, Hexane and diisopropyl ether were added to the obtained residue and a solid substance was separated by filtration to obtain 0.29 g of methyl 2-(benzamido)-4-((phenylthio)methyl)benzoate as white solid.

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