HRID1678845

反应详情

EQUATION

反应方程式

HRID 1678845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4a-(m-Methoxyphenyl)-1,3-diketo-1,2,3,4,4a,5,6,7-octahydroisoquinoline (6 g) in 75 ml of anhydrous dimethylformamide was added to a 55% suspension of sodium hydride in mineral oil (1.2 g) in 50 ml of dimethylformamide at 70°. The reaction mixture was heated for one hour at 80° and then cooled to 25°. p-Methylphenethyl mesylate (7.0 g) was added and the reaction heated at 70° for 18 hours. It was poured into water and extracted with ether. The residue after evaporation of the ether was chromatographed on 800 g. of Florisil. This yielded 4.4 g, mp 134°-140°; recrystallized from ethanol, mp 149°-151°.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated for one hour at 80°
  2. temperaturecooled to 25°
  3. temperaturethe reaction heated at 70° for 18 hours
  4. extractionextracted with ether
  5. customThe residue after evaporation of the ether
  6. customwas chromatographed on 800 g
  7. customrecrystallized from ethanol, mp 149°-151°