HRID606455
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
- 90 °C
PROCEDURE
实验过程
A suspension of 3-(1H-1,2,4-triazol-3-yl)propanoic acid obtained in Reference Example 22 (11.6 g, 3.54 mmol) and 2N hydrogen chloride/ethanol (100 mL) in ethanol (100 mL) was stirred at 90° C. for 15 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was extracted with ethyl acetate and water. The aqueous layer was neutralized with saturated aqueous sodium carbonate solution, and the organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated to give the title compound as a yellow powder (4.36 g, 33%).
WORKUP
后处理
- filtrationThe insoluble material was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- extractionThe residue was extracted with ethyl acetate and water
- washthe organic layer was washed with saturated brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated