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
PROCEDURE
实验过程
To 18.58 g of 5-phenylsalicylic acid, 350 ml of ethanol, 100 ml of toluene and 42 ml of concentrated sulfuric acid were added. The mixture was heated under reflux for 14 hours. After it was confirmed with TLC that the starting materials were almost disappeared, the reaction liquid was poured into a mixed medium of diluted hydrochloric acid-ethyl acetate. The mixture was extracted, and the organic phase was collected and washed with saturated sodium chloride aqueous solution. After dried with magnesium sulfate, the liquid was concentrated to form a crude product. The product was recrystallized from ethanol to obtain 11.53 g of ethyl 5-phenylsalicylate in the form of colorless crystallites. The yield was 55%. The product was confirmed with NMR and mass spectroscopy.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 14 hours
- customthe reaction liquid
- extractionThe mixture was extracted
- customthe organic phase was collected
- washwashed with saturated sodium chloride aqueous solution
- dry with materialAfter dried with magnesium sulfate
- concentrationthe liquid was concentrated
- customto form a crude product
- customThe product was recrystallized from ethanol