HRID1850053
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture was then evaporated under reduced pressure and water (10 mL)
- additionwas added to the residue
- customThe carboxylic acid precipitated
- extractionwas extracted with ethyl acetate
- washThe EtOAc layer was washed with water (2×10 mL) and brine (1×15 mL)
- dry with materialIt was dried over sodium sulfate
- filtrationfiltered
- customevaporated under vacuum