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
A mixture of (±)-6-[[4-(chloromethyl)phenyl]hydroxy(1-methyl-1H-imidazol-5-yl)methyl]-4-(3-chlorophenyl)-1-methyl-2(1H)-quinolinone (0.0002 mol), obtained in Example B14, and 2(3H)-thiazolethione (0.001 mol) in THF (1 ml) and triethylamine (0.1 ml) was stirred at room temperature for 18 hours, poured out into water and extracted with CH2Cl2/CH3OH. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated. The residue was purified by column chromatography over kromasil 60 μm (eluent: CH2Cl2/CH3OH; 90/10). The pure fractions were collected and the solvent was evaporated, yielding (70%) of 4(3-chlorophenyl)-6-[hydroxy(1-methyl-1H-imidazol-5-yl)[4-[(2-thiazolylthio)methyl]phenyl]methyl]-1-methyl-2(1H)-quinolinone, as a white foam, MS (ESI) m/z:585, 586 (MH+).
WORKUP
后处理
- extractionextracted with CH2Cl2/CH3OH
- customThe organic layer was separated
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent was evaporated
- customThe residue was purified by column chromatography over kromasil 60 μm (eluent: CH2Cl2/CH3OH; 90/10)
- customThe pure fractions were collected
- customthe solvent was evaporated