HRID1395090

反应详情

EQUATION

反应方程式

HRID 1395090 的结构方程式

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A mixture of 92.5 g monochloroacetone (1 mole) and 93 g of α-picoline (1 mole) was heated for 21/2 h on a boiling water-bath. The reaction mixture was cooled to ambient temperature (20° C.) and kept overnight. A solid black mass formed. Extraction was performed on a hot water-bath until the mass had dissolved completely (about 700 ml). The solution was filtered and washed 3 times with 100 ml of ether. A few ml of an aqueous saturated sodium carbonate solution were added and the solution was then washed again 4 times in ether. 150 g of solid sodium hydrogen carbonate was added carefully and steam distillation was carried out. The distillate was cooled and sucked off. The solid product was dissolved quickly in ether and dried on heated magnesium sulphate. The ether was evaporated and the residue dried.

WORKUP

后处理

  1. temperaturewas heated for 21/2 h on a boiling water-bath
  2. customA solid black mass formed
  3. extractionExtraction
  4. customwas performed on a hot water-bath until the mass
  5. dissolutionhad dissolved completely (about 700 ml)
  6. filtrationThe solution was filtered
  7. washwashed 3 times with 100 ml of ether
  8. additionA few ml of an aqueous saturated sodium carbonate solution were added
  9. washthe solution was then washed again 4 times in ether
  10. addition150 g of solid sodium hydrogen carbonate was added carefully
  11. distillationsteam distillation
  12. temperatureThe distillate was cooled
  13. dissolutionThe solid product was dissolved quickly in ether
  14. customdried
  15. temperatureon heated magnesium sulphate
  16. customThe ether was evaporated
  17. customthe residue dried