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
1.7 g of ethyl (Z)-2-(2-acetamidothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetate are suspended in 17 ml of methanol, and 5 ml of 2N sodium hydroxide are added thereto. The mixture is refluxed for 30 minutes with heating. Then, the mixture is concentrated under reduced pressure to remove methanol. The residue is adjusted to pH 2 with diluted hydrochloric acid, and the aqueous mixture is extracted with a mixture of ethyl acetate and tetrahydrofuran (2:1). The extract is dried and concentrated under reduced pressure to dryness. The residue is crystallized with isopropanol, and the crystals are collected by filtration and then recrystallized from water. 0.8 g of (Z)-2-(2-acetamidothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetic acid is obtained.
WORKUP
后处理
- temperatureThe mixture is refluxed for 30 minutes
- temperaturewith heating
- concentrationThen, the mixture is concentrated under reduced pressure
- customto remove methanol
- extractionthe aqueous mixture is extracted with a mixture of ethyl acetate and tetrahydrofuran (2:1)
- customThe extract is dried
- concentrationconcentrated under reduced pressure to dryness
- customThe residue is crystallized with isopropanol
- filtrationthe crystals are collected by filtration
- customrecrystallized from water