HRID1156898

反应详情

EQUATION

反应方程式

HRID 1156898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(p-Toluoylamino)-2-(2-chlorophenyl)ethane (70 g) was dissolved in 700 ml of xylene and 320 ml of phosphorus oxychloride, and while the solution was heated with stirring, 240 g of phosphorus pentoxide was added. The mixture was heated under reflux for 4 hours. Water was added to the reaction mixture. The aqueous layer was made weakly alkaline with an aqueous solution of sodium hydroxide, extracted with benzene, washed in water, and dried. The solvent was distilled off, and the residue was recrystallized from benzene to afford 29 g of 1-(4-methylphenyl)-5-chloro-3,4-dihydroisoquinoline as colorless needles.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. extractionextracted with benzene
  4. washwashed in water
  5. customdried
  6. distillationThe solvent was distilled off
  7. customthe residue was recrystallized from benzene