HRID1717327

反应详情

EQUATION

反应方程式

HRID 1717327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 3-hydroxy-4-nitrobenzoic acid (9.16 g) in DMF (100 ml) were successively added 2M ethylamine in THF solution (30 ml), triethylamine (8.3 ml), HOBt (9.19 g) and WSC (11.5 g), and the reaction mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure, ethyl acetate and 1N hydrochloric acid were added to the residue and the insoluble material was filtered off. The filtrate was extracted with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound as a yellow solid (10.6 g, 100%).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure, ethyl acetate and 1N hydrochloric acid
  2. additionwere added to the residue
  3. filtrationthe insoluble material was filtered off
  4. extractionThe filtrate was extracted with ethyl acetate
  5. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure