HRID2071119

反应详情

EQUATION

反应方程式

HRID 2071119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Dimethyl 5-(N-methylmethylsulfonamido)isophthalate (0.842 g, 2.8 mmol) was dissolved in THF:MeOH (1:1) (8 mL) and H2O (3 mL). Solid NaOH (0.112 g, 2.8 mmol) was added and stirred at room temperature for 18 h. The reaction mixture was concentrated under reduced pressure. Saturated NaHCO3 (10 mL) was added to the reaction mixture and extracted with toluene (to remove <10% unreacted starting material). The aqueous solution was acidified with dilute HCl (10%), extracted with EtOAc, and dried over anhydrous Na2SO4. The solvent was evaporated and dried under reduced pressure to give 3-(methoxycarbonyl)-5-(N-methylmethylsulfonamido)benzoic acid as a white solid (75%, 0.598 g), which was used without further purification.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionSaturated NaHCO3 (10 mL) was added to the reaction mixture
  3. extractionextracted with toluene (to remove <10% unreacted starting material)
  4. extractionextracted with EtOAc
  5. dry with materialdried over anhydrous Na2SO4
  6. customThe solvent was evaporated
  7. customdried under reduced pressure