HRID461295

反应详情

EQUATION

反应方程式

HRID 461295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 0.18 mole of 4-methoxy-phenylhydrazine, 0.27 mole of methyl isopropylketone, 5 drops of acetic acid and 300 ml of ethanol was refluxed for 3 h, whereupon the solvent was evaporated. The dark residue (28 g of hydrazone) was dissolved in 125 ml of ethanol. After adding 54 ml of a 15% by weight solution of concentrated sulphuric acid in ethanol the mixture was refluxed for 2.5 h. The white precipitate (ammonium sulphate) was filtered and the filtrate was diluted with 750 ml of water, neutralized with a few ml of aqueous 5N sodium hydroxide and extracted with ether. The dried extract was distilled in vacuo. Boiling point: 138°-142° C/8 mm Hg.

WORKUP

后处理

  1. temperaturewas refluxed for 3 h, whereupon the solvent
  2. customwas evaporated
  3. dissolutionThe dark residue (28 g of hydrazone) was dissolved in 125 ml of ethanol
  4. additionAfter adding 54 ml of a 15% by weight solution of concentrated sulphuric acid in ethanol the mixture
  5. temperaturewas refluxed for 2.5 h
  6. filtrationThe white precipitate (ammonium sulphate) was filtered
  7. additionthe filtrate was diluted with 750 ml of water
  8. extractionextracted with ether
  9. extractionThe dried extract
  10. distillationwas distilled in vacuo