HRID852274

反应详情

EQUATION

反应方程式

HRID 852274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Methyl iodide (1.58 ml) was added to a solution of interm. (5-f) (7.6 g) and benzyl-triethylammonium chloride (BTEAC) (2.23 g) in THF (80 ml) and sodium hydroxide (40%, 80 ml). The mixture was stirred at room temperature for 2 hours. Water was added and the mixture was extracted with ethyl acetate. The organic layer was dried, filtered, and the solvent was evaporated. The residue was purified by flash column chromatography over silica gel (eluent: DCM 100%). The desired fractions were collected and the solvent was evaporated, yielding 7.1 g (90%) of 6-(4-chlorobenzoyl)-4-(3-methoxyphenyl)-1-methyl-2(1H)-quinolinone (interm. 5-g).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe organic layer was dried
  3. filtrationfiltered
  4. customthe solvent was evaporated
  5. customThe residue was purified by flash column chromatography over silica gel (eluent: DCM 100%)
  6. customThe desired fractions were collected
  7. customthe solvent was evaporated