HRID481404

反应详情

EQUATION

反应方程式

HRID 481404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Triethylorthoformate (1.5 ml) and 1-(6-methylnaphthalen-2-yl)ethanone (1.0 mmol) were dissolved in ethanol (4 ml). To the reaction mixture were added AgNO3 (2.1 mmol) and I2 (1.05 mmol) and the reaction mixture was heated to 80° C. for 20 hours. The reaction mixture was cooled to ambient temperature and concentrated to dryness. The residue was diluted eith EtOAc and filtered through celite. The combined organics were washed with saturated sodium bicarbonate solution and brine. The organic layer was then dried over MgSO4, filtered and concentrated to dryness. The crude residue was chromatographed on silica gel using 5% EtOAc in hexanes as the eluant to yield the title compound (50).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to ambient temperature
  2. concentrationconcentrated to dryness
  3. additionThe residue was diluted eith EtOAc
  4. filtrationfiltered through celite
  5. washThe combined organics were washed with saturated sodium bicarbonate solution and brine
  6. dry with materialThe organic layer was then dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated to dryness
  9. customThe crude residue was chromatographed on silica gel using 5% EtOAc in hexanes as the eluant