HRID1288229

反应详情

EQUATION

反应方程式

HRID 1288229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of phenol (18.8 g.) and anhydrous potassium carbonate (25 g.) in dry ethyl methyl ketone (35 ml.) was stirred and heated to reflux, during the dropwise addition of a solution of 2-chloropropionitrile (19.7 g.) in dry ethyl methyl ketone (15 ml.) containing finely-powdered potassium iodide (0.5 g.). The addition took 20 minutes. Stirring and heating were continued for a total of 2 hours after which the mixture was cooled, poured into water (200 ml.) and extracted with ether (200, 75 and 75 ml.). The combined ether extract was washed several times with 2N-sodium hydroxide to remove phenol, dried over anhydrous sodium sulphate, and evaporated. The residue was distilled under water-pump vacuum to give pure 2-phenoxypropionitrile, b.p. 117°-118°/13 mm.

WORKUP

后处理

  1. temperatureheated
  2. additionThe addition
  3. stirringStirring
  4. temperatureheating
  5. customwere continued for a total of 2 hours
  6. temperaturewas cooled
  7. extractionextracted with ether (200, 75 and 75 ml.)
  8. extractionThe combined ether extract
  9. washwas washed several times with 2N-sodium hydroxide
  10. customto remove phenol
  11. dry with materialdried over anhydrous sodium sulphate
  12. customevaporated
  13. distillationThe residue was distilled under water-pump vacuum