反应详情

To a solution of 38.5 g (0.15 mole) of N-[2-(4-fluorophenylthio]ethyl-1-methyl-ethanamine and 15.5 g (0.15 mole) of triethylamine in 300 ml of methylene chloride which was cooled in an ice bath was added dropwise with stirring a solution of 23.5 g (0.15 mole) of phenyl chloroformate in 100 ml of methylene chloride over a 15 minute period. The resulting solution was stirred overnight at room temperature and extracted with 5% aqueous sodium hydroxide. The chloroform layer was dried and filtered and evaporated to give an oil residue which crystallized to a white solid. A portion of the solid was triturated with isopropyl ether and the mixture cooled under refrigeration. The solid was collected by filtration and dried in vacuo overnight at 80° C. White crystalline product, m.p. 53°-58° C. was obtained.

1. additionwas added dropwise
2. extractionextracted with 5% aqueous sodium hydroxide
3. dry with materialThe chloroform layer was dried
4. filtrationfiltered
5. customevaporated
6. customto give an oil residue which
7. customcrystallized to a white solid
8. customA portion of the solid was triturated with isopropyl ether
9. temperaturethe mixture cooled under refrigeration
10. filtrationThe solid was collected by filtration
11. customdried in vacuo overnight at 80° C
12. customWhite crystalline product, m.p. 53°-58° C. was obtained