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
- 25 °C
PROCEDURE
实验过程
A mixture of 2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4,4-difluoro-butyric acid methyl ester (790 mg, 2.28 mmol) in a 1:1 solution of tetrahydrofuran:water (20 mL) was treated with lithium hydroxide monohydrate (230 mg, 4.56 mmol). The mixture was stirred for 2 h at 25° C. After such time, the mixture was concentrated in vacuo to remove the tetrahydrofuran and then diluted with water, and the pH adjusted to pH=5 with 1N aqueous hydrochloric acid and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated in vacuo to afford 2-[4-(2-chloro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4,4-difluoro-butyric acid (571 mg, 75%) as a cream colored solid: HR-ES-MS m/z calculated for C14H12NO4ClF2 [M+H]+ 332.0496, observed 332.0496.
WORKUP
后处理
- concentrationAfter such time, the mixture was concentrated in vacuo
- customto remove the tetrahydrofuran
- additiondiluted with water
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo