HRID1047951

反应详情

EQUATION

反应方程式

HRID 1047951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4,5-Difluoro-2-[3-methyl-2-(2-methyl-propenyl)-benzoylamino]-indan-2-carboxylic acid ethyl ester (387) (650 mg, 1.57 mmol) is dissolved in EtOH (50 mL) and set to stir at RT. To this solution is added 5M KOH (4 mL). The reaction mixture is stirred at RT overnight. After concentration in vacuo, the residue obtained is dissolved in water (20 mL) and washed with EtOAc (20 mL). The phases are separated and the aqueous phase is acidified with concentrated HCl to pH 2. The solid precipitate is collected via filtration, dried under vacuum, and then purified on an HPLC. The desired product (388) is obtained as white solid (440.0 mg, 73%).

WORKUP

后处理

  1. stirringThe reaction mixture is stirred at RT overnight
  2. concentrationAfter concentration in vacuo
  3. customthe residue obtained
  4. washwashed with EtOAc (20 mL)
  5. customThe phases are separated
  6. filtrationThe solid precipitate is collected via filtration
  7. customdried under vacuum
  8. custompurified on an HPLC