HRID1469642

反应详情

EQUATION

反应方程式

HRID 1469642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-chloroisophthalic acid dimethyl ester (457 mg, 2 mmol) in methanol (10 mL) is added aqueous 1M NaOH (1.0 mL, 0.65 mmol) and the mixture is stirred at room temperature for 18 hours. The solvent is removed under reduced pressure and water is added to the residue. The solution is washed with ethyl acetate and the aqueous phase is acidified with aqueous 1M HCl. The mixture is extracted with ethyl acetate and the organic phase is washed with brine and dried over sodium sulfate. The solvent is removed under reduced pressure to give the title compound. MS 213.2 (M−1); 1H-NMR (400 MHz, DMSO-d6); δ ppm 3.91 (s, 3H), 8.15 (s, 2H), 8.38 (s, 1H), 13.71 (s, 1H).

WORKUP

后处理

  1. customThe solvent is removed under reduced pressure and water
  2. additionis added to the residue
  3. washThe solution is washed with ethyl acetate
  4. extractionThe mixture is extracted with ethyl acetate
  5. washthe organic phase is washed with brine
  6. dry with materialdried over sodium sulfate
  7. customThe solvent is removed under reduced pressure