HRID1156863
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 30 g of 1-(4-chlorophenyl)-5-methyl-3,4-dihydroisoquinoline and 30 g of diphenyl disulfide was dissolved in 800 ml of tetralin, and the solution was heated. After the reaction, the tetralin was distilled off under reduced pressure. The residue was dissolved in benzene, and extracted with a 2 N aqueous solution of hydrochloric acid. The aqueous layer was neutralized with an aqueous solution of sodium hydroxide, extracted with ether, and dried, followed by distilling off the solvent. Recrystallization of the residue from benzenecyclohexane afforded 18 g of 1-(4-chlorophenyl)-5-methylisoquinoline as colorless needles having a melting point of 122° to 123.5° C.
WORKUP
后处理
- temperaturethe solution was heated
- customAfter the reaction
- distillationthe tetralin was distilled off under reduced pressure
- dissolutionThe residue was dissolved in benzene
- extractionextracted with a 2 N aqueous solution of hydrochloric acid
- extractionextracted with ether
- customdried
- distillationby distilling off the solvent
- customRecrystallization of the residue from benzenecyclohexane