HRID409254

反应详情

EQUATION

反应方程式

HRID 409254 的结构方程式

PROCEDURE

实验过程

To a solution of [5-(2-Ethyl-6-methyl-phenoxy)-1,3-dioxo-1,3-dihydro-isoindol-2-yl]-acetic acid methyl ester (22 mmol, 7.77 g) in anhydrous n-butanol (150 mL) was added a 1 N solution of sodium in n-butanol (45 mmol, 45 mL) at 95° C. in one portion with stirring. Stirring was continued at 95° C. for 3 h before the mixture was concentrated in vacuo. To the residue was added 2 N hydrochloric acid (60 mmol, 30 mL) and EtOAc (150 mL) and the mixture was stirred vigorously for 45 min. Subsequently, the solid component was sucked off, washed with water and dried in vacuo to give the title compound as a tan solid (623 mg); MS-(+)-ion: M+1=396.5.

WORKUP

后处理

  1. stirringStirring
  2. concentrationwas concentrated in vacuo
  3. stirringthe mixture was stirred vigorously for 45 min
  4. washwashed with water
  5. customdried in vacuo