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
- 201.5 °C
PROCEDURE
实验过程
5.40 g (14.3 m mole) of 2-(6-acetoxy-2-naphthoylamino)-4-butylphenol, 0.43 g of p-toluenesulfuric acid monohydrate and 40 ml of O-dichlorobenzene were placed in a 100 ml round-bottom flask, followed by heating and stirring for 30 minutes at 200-203° C. After the reaction, O-dichlorobenzene was distilled off under reduced pressure. To the resultant, 2.00 g (30.3 m mole) of potassium hydroxide and 60 ml of ethanol were added, followed by heating and stirring for 20 minutes at 60° C. After the reaction, the reaction mixture was poured into 600 ml of water. To the reaction mixture, 8 ml of chloric acid was added to precipitate a crystal. The crystal was filtered, washed with water and recrystallized from a mixture solvent of acetoneethanol to obtain 2.18 g of 2-(6-hydroxy-2-naphthyl)-5-butylbenzooxazole (Yield: 42.4%).
WORKUP
后处理
- temperatureby heating
- distillationwas distilled off under reduced pressure
- additionTo the resultant, 2.00 g (30.3 m mole) of potassium hydroxide and 60 ml of ethanol were added
- temperatureby heating
- stirringstirring for 20 minutes at 60° C
- customAfter the reaction
- customto precipitate a crystal
- filtrationThe crystal was filtered
- washwashed with water
- customrecrystallized from a mixture solvent of acetoneethanol