HRID2268533
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 mixture of N, N-dimethyl-4-[3-(4,5,6,7-tetramethoxyindan-2-yl)propoxy]benzamide (700 mg), 2,6-pyridinedicarboxylic acid (792 mg), THF (14 ml), and water (7 ml) was dropwise added a solution of CAN (3.44 g) in water (7 ml) with cooling with ice. After the reaction mixture was stirred for 15 min, water was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, and dried. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (ethyl acetate) and then with recrystallization from hexane-ethyl acetate to yield the entitled compound (438 mg) as crystals.
WORKUP
后处理
- temperaturewith cooling with ice
- extractionwas extracted with ethyl acetate
- washThe organic layer was washed with water and saturated aqueous sodium chloride
- customdried
- customThe solvent was removed in vacuo
- customThe residue was purified by silica gel column chromatography (ethyl acetate)
- customwith recrystallization from hexane-ethyl acetate