HRID376894

反应详情

EQUATION

反应方程式

HRID 376894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A suspension of 60.8 g potassium carbonate in 300 ml of dry pyridine was treated with 35.7 g 7-hydroxy-3,4-dihydro-2H-naphthalen-1-one, and the mixture was heated to 40° C. Thereafter, 19.9 g copper(II) oxide was added thereto with stirring, followed by the drop-wise addition of 39.6 g bromobenzene. The reaction mixture was heated for 4 days under reflux. After evaporating the pyridine completely under vacuum, the residue was stirred with 200 ml ethyl acetate and was filtered through silica gel. The filtrate was washed with saturated solutions of ammonium chloride and sodium chloride, dried over sodium sulfate and concentrated by evaporation under vacuum. The residue was purified by column chromatography, using n-hexane/ethyl acetate as the elutant, whereupon 41.2 g (78.6% of theoretical) 7-phenoxy-3,4-dihydro-2H-naphthalen-1-one was obtained.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated for 4 days
  2. temperatureunder reflux
  3. customAfter evaporating the pyridine completely under vacuum
  4. stirringthe residue was stirred with 200 ml ethyl acetate
  5. filtrationwas filtered through silica gel
  6. washThe filtrate was washed with saturated solutions of ammonium chloride and sodium chloride
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated by evaporation under vacuum
  9. customThe residue was purified by column chromatography