反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of methyl 4,5-diphenyl-2-oxazoleoctanoate (7.00 g, 18.5 mmol), 5N sodium hydroxide solution (7.42 mL), water (100 mL) and methanol (20 mL) was heated on a steam bath for 45 minutes. After stirring at room temperature for 75 minutes, the mixture was diluted with water (150 mL), heated on a steam bath for 10 minutes and then allowed to stir overnight at room temperature. The mixture was heated to reflux for 1 hour, cooled, acidified with 2N hydrochloric acid solution and extracted with CH2Cl2. The combined extracts were dried over sodium sulfate and concentrated in vacuo to give an oil that crystallized. Recrystallization from a mixture of diethyl ether, CH2Cl2 and hexanes furnished 4,5-diphenyl-2-ozazoleoctanoic acid (5.25 g, 77%), m.p. 70°-73° C.
WORKUP
后处理
- temperaturewas heated on a steam bath for 45 minutes
- temperatureheated on a steam bath for 10 minutes
- stirringto stir overnight at room temperature
- temperatureThe mixture was heated
- temperatureto reflux for 1 hour
- temperaturecooled
- extractionextracted with CH2Cl2
- dry with materialThe combined extracts were dried over sodium sulfate
- concentrationconcentrated in vacuo
- customto give an oil
- customthat crystallized
- customRecrystallization
- additionfrom a mixture of diethyl ether, CH2Cl2 and hexanes
- customfurnished 4,5-diphenyl-2-ozazoleoctanoic acid (5.25 g, 77%), m.p. 70°-73° C.