HRID1436682
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
Chill a solution of N-methyl-N-propyl-5-(pyridine-3-carbonyl)-isophthalamic acid methyl ester (0.070 g, 0.206 mmol) in MeOH (1 mL) and THF (1 mL) in an ice bath. Add 1 N NaOH (0.62 mL, 0.62 mmol) and stir at room temperature for 2 h. Acidify the solution to about pH=2 and concentrate to one half of the solvent. Partition the residue between ethyl acetate and H2O. Extract the aqueous layer with ethyl acetate (2×15 mL). Wash the combined organic extract with saturated aqueous sodium chloride, dry (magnesium sulfate) and concentrate to give the title compound (72%).
WORKUP
后处理
- concentrationconcentrate to one half of the solvent
- customPartition the residue between ethyl acetate and H2O
- extractionExtract the aqueous layer with ethyl acetate (2×15 mL)
- washWash the combined
- extractionorganic extract with saturated aqueous sodium chloride
- dry with materialdry (magnesium sulfate)
- concentrationconcentrate