HRID1850053

反应详情

EQUATION

反应方程式

HRID 1850053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

(E)-methyl 3-(1-methyl-1H-pyrazol-4-yl)acrylate (0.24 g, 1.45 mmol) was dissolved in MeOH (10 mL). A 1M solution of KOH (5.8 mL) was added and the mixture was heated at 70° C. overnight. The reaction mixture was then evaporated under reduced pressure and water (10 mL) was added to the residue. This solution was carefully acidified to pH 4 with a 3M aqueous solution of HCl. The carboxylic acid precipitated and was extracted with ethyl acetate. The EtOAc layer was washed with water (2×10 mL) and brine (1×15 mL). It was dried over sodium sulfate, filtered and evaporated under vacuum to give (E)-3-(1-methyl-1H-pyrazol-4-yl)acrylic acid as a white solid (160 mg). ES+(M+H)+153

WORKUP

后处理

  1. customThe reaction mixture was then evaporated under reduced pressure and water (10 mL)
  2. additionwas added to the residue
  3. customThe carboxylic acid precipitated
  4. extractionwas extracted with ethyl acetate
  5. washThe EtOAc layer was washed with water (2×10 mL) and brine (1×15 mL)
  6. dry with materialIt was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated under vacuum