HRID413696
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
To a solution of 3-(5-phenyl-benzofuran-2-ylmethoxycarbonylamino)-isonicotinic acid ethyl ester (0.150 g, 0.36 mmol) in THF (3 ml) was added at room temperature 1.0M LiOH (0.72 mL, 0.72 mmol) and the mixture was stirred for 3 h. The solvent was evaporated, water was added, followed by 2N HCl to adjust the pH to 1-2, and the product was extracted with EtOAc. The extract was washed with water, then brine, and dried over magnesium sulfate and concentrated to dryness. Purification by crystallization gave 0.072 g of 3-(5-phenyl-benzofuran-2-ylmethoxycarbonylamino)-isonicotinic acid as a white solid, mp 235.7-238.9° C.
WORKUP
后处理
- customThe solvent was evaporated
- additionwater was added
- extractionthe product was extracted with EtOAc
- washThe extract was washed with water
- dry with materialbrine, and dried over magnesium sulfate
- concentrationconcentrated to dryness
- customPurification
- customby crystallization