HRID1414950

反应详情

EQUATION

反应方程式

HRID 1414950 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add mercuric sulphate (0.45 g) to a stirred solution of 1-diethylamino-5-methyl-6-(m-methoxyphenyl)hex-2-yne (8 g) in concentrated sulfuric acid (2.5 cc) and water (25 cc) and heat the mixture at 70° for 11/2 hours. Filter the cooled solution, make basic with 10% aqueous sodium hydroxide and extract with ether. Wash and dry the ethereal solution and evaporate to leave as residue crude 1-diethylamino-6-(m-methoxyphenyl)-5-methylhexan-3-one; infrared absorption peaks at 5.85 μ. Slowly distil at 0.1 mm Hg to obtain 5-methyl-6-(m-methoxyphenyl)hex-1-en-3-one; infrared absorption peaks at 5.85 μ.

WORKUP

后处理

  1. temperatureheat the mixture at 70° for 11/2 hours
  2. filtrationFilter the cooled solution
  3. extractionextract with ether
  4. washWash
  5. customdry the ethereal solution
  6. customevaporate
  7. customto leave as residue crude 1-diethylamino-6-(m-methoxyphenyl)-5-methylhexan-3-one
  8. custominfrared absorption peaks at 5.85 μ
  9. customSlowly distil at 0.1 mm Hg