HRID2261296

反应详情

EQUATION

反应方程式

HRID 2261296 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

18.68 g of methyl 2-(dimethoxymethyl)-3-hydroxyacrylate sodium salt was added to 80 ml of ethanol, and 18.39 g of benzylhydrazine dihydrochloride was added. The mixture was stirred at 70° C. for 7 hours and then cooled to room temperature. After 100 ml of water was added, the mixture was concentrated to 100 ml under reduced pressure. The concentrated solution was extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 7.39 g of methyl 1-benzyl-1H-pyrazole-4-carboxylate.

WORKUP

后处理

  1. additionwas added
  2. temperaturecooled to room temperature
  3. concentrationthe mixture was concentrated to 100 ml under reduced pressure
  4. extractionThe concentrated solution was extracted with ethyl acetate
  5. washThe organic layer was washed with aqueous saturated sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure