HRID2241119

反应详情

EQUATION

反应方程式

HRID 2241119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Ethyl 3-cyano-2,4,5-trifluorobenzoate (3.35 g, 14.6 mmol) was suspended in glacial acetic acid (5 mL). Concentrated hydrochloric acid (10 mL) was added thereto, and the mixture was stirred at 100° C. for 4 hours. While cooling with ice, water (100 mL) was added to the reaction mixture. Subsequently, the resultant mixture was extracted with chloroform (100 mL×4), followed by drying with sodium sulfate anhydrate. After filtration, the filtrate was concentrated under reduced pressure. The residue was recrystallized from chloroform/n-hexane, to thereby yield the title compound as a white solid (2.86 g, 97%).

WORKUP

后处理

  1. additionwas added to the reaction mixture
  2. extractionSubsequently, the resultant mixture was extracted with chloroform (100 mL×4)
  3. dry with materialby drying with sodium sulfate anhydrate
  4. filtrationAfter filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was recrystallized from chloroform/n-hexane