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
N-[3-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-(3-pyridyl)benzoyl]piperidine (80 mg, 0.1632 mmol) was dissolved in a mixed solvent of acetonitrile (9 ml) and water (3 ml), then CAN (128 mg, 0.2335 mmol) was added thereto at room temperature and the mixture was stirred for 1 hour. The reaction solution poured into water, neutralized with a saturated aqueous solution of sodium hydrogen carbonate and extracted with ethyl acetate. The extract was washed with water and dried and the solvent was evaporated therefrom. The residue was purified by preparative thin layer silica gel (hexane:ethyl acetate=1:3) to give the title compound (51 mg, 0.1108 mmol, 68%). This compound was converted to a methanesulfonate by the method according to Example 58.
WORKUP
后处理
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- customdried
- customthe solvent was evaporated
- customThe residue was purified by preparative thin layer silica gel (hexane:ethyl acetate=1:3)