HRID1081290

反应详情

EQUATION

反应方程式

HRID 1081290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11 g of pyrocatechol were dissolved in 200 ml of dimethylfomamide, and 18 g of 45% strength by weight aqueous sodium hydroxide solution were added. 20 g of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene were added dropwise at 75° C. to the mixture. Stirring was continued for 30 minutes at 75° C. The mixture was then poured into 500 ml of ice-water and extracted with diethyl ether. The organic phase was washed with water, dried with magnesium sulphate and concentrated. Finally, the product was distilled under a high vacuum. The yield was 15 g (=56%) the boiling point was 60° C. at 10 mbar. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -59.0 and -84.6 ppm; 1H-NMR: 3.02 ppm.

WORKUP

后处理

  1. additionwere added
  2. extractionextracted with diethyl ether
  3. washThe organic phase was washed with water
  4. dry with materialdried with magnesium sulphate
  5. concentrationconcentrated
  6. distillationFinally, the product was distilled under a high vacuum