HRID2268533

反应详情

EQUATION

反应方程式

HRID 2268533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewith cooling with ice
  2. extractionwas extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous sodium chloride
  4. customdried
  5. customThe solvent was removed in vacuo
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  7. customwith recrystallization from hexane-ethyl acetate