HRID1039114

反应详情

EQUATION

反应方程式

HRID 1039114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

19.9 g Dichloromethyl methyl ether and 45.7 g tin chloride were dissolved in 70 ml dichloromethane. The solution was cooled to +5° C. and 20.0 g fluoronapthalene in dichloromethane (49 ml) was added over a 60 min period, while keeping the temperature at 5° C. The reaction was brought to room temperature after the addition. After 4 h the reaction was quenched by slowly pouring it into an ice/water mixture. This mixture was stirred for 15 min and left standing overnight. The dichloromethane layer was washed with water, dried (sodium sulphate), filtered through celite and concentrated in vacuo to obtain 24.0 g of 4-fluoro-naphthalene-1-carbaldehyde as an off white solid.

WORKUP

后处理

  1. temperatureThe solution was cooled to +5° C.
  2. customat 5° C
  3. customwas brought to room temperature
  4. additionafter the addition
  5. customAfter 4 h the reaction was quenched
  6. additionby slowly pouring it into an ice/water mixture
  7. waitleft
  8. waitstanding overnight
  9. washThe dichloromethane layer was washed with water
  10. dry with materialdried (sodium sulphate)
  11. filtrationfiltered through celite and
  12. concentrationconcentrated in vacuo