HRID1156899

反应详情

EQUATION

反应方程式

HRID 1156899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(4-Methylphenyl)-5-chloro-3,4-dihydroisoquinoline (29 g) and 24.7 g of diphenyl disulfide were reacted over an oil bath at 220° C. The reaction mixture was dissolved in cyclohexane, and extracted with a 4 N aqueous solution of hydrochloric acid. The aqueous layer was neutralized with an aqueous solution of sodium hydroxide. The resulting oily product was extracted with benzene, washed in water, and dried. The solvent was distilled off, and the residue was recrystallized from benzene to afford 22.5 g of 1-(4-methylphenyl)-5-chloroisoquinoline as colorless needles having a melting point of 88.6° to 89.1° C.

WORKUP

后处理

  1. extractionextracted with a 4 N aqueous solution of hydrochloric acid
  2. extractionThe resulting oily product was extracted with benzene
  3. washwashed in water
  4. customdried
  5. distillationThe solvent was distilled off
  6. customthe residue was recrystallized from benzene