HRID1450647
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
Added to 500 g (4.2 mol) of thionyl chloride were 110 g (0.58 mol) of 3-phenylisoxazole-5-carboxylic acid prepared above in the procedure (2), followed by the further addition of 2 ml of dimethylformamide. The resulting mixture was heated under reflux for 3 hours. After completion of the reaction, thionyl chloride was distilled off under reduced pressure, followed by the addition of 500 ml of benzene. When the mixture thus obtained was distilled under reduced pressure, the title compound, i.e., 3-phenylisoxazole-5-carboxylic acid chloride was obtained as a solid. It was provided for the next step without purification.
WORKUP
后处理
- customprepared above in the procedure (2)
- temperatureThe resulting mixture was heated
- temperatureunder reflux for 3 hours
- distillationwas distilled off under reduced pressure
- additionfollowed by the addition of 500 ml of benzene
- customWhen the mixture thus obtained
- distillationwas distilled under reduced pressure