反应详情

To a solution of 22.8 g (0.1 mole) of N-[2-[(4-chlorophenyl)thio]ethyl]-1-methylethanamine (oil in Preparation 1) and 10.1 g (0.1 mole) of triethylamine in 300 ml of methylene chloride was added dropwise with stirring a solution of 15.7 g (0.1 mole) phenyl chloroformate in 100 ml of methylene chloride. The resulting solution was stirred overnight at room temperature. The methylene chloride layer was extracted with 5% sodium hydroxide solution followed by 1N sulfuric acid. The methylene chloride layer was concentrated to give an oil which crystallized to a white solid. Recrystallization from isopropyl ether gave white crystalline product, m.p. 54°-56° C. in 79.6% yield.

1. extractionThe methylene chloride layer was extracted with 5% sodium hydroxide solution
2. concentrationThe methylene chloride layer was concentrated
3. customto give an oil which
4. customcrystallized to a white solid
5. customRecrystallization from isopropyl ether
6. customgave white crystalline product, m.p. 54°-56° C. in 79.6% yield