反应详情

A mixture of 8.30 g (44.5 mmols) of 1-chloro-3-phenylthiopropane, 100 ml of diethanolamine, 13.3 g (88.7 mmols) of sodium iodide and 250 ml of dioxan was heated under reflux for 15 hours. The mixture was concentrated under reduced pressure, and an aqueous saturated sodium bicarbonate solution was added to the mixture followed by extraction of the solution with chloroform 5 times. The chloroform layer was drided over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: chloroform/methanol =25/1) to afford 6.46 g (yield: 57%) of 1-bis(hydroxyethyl)amino-3-phenylthiopropane.

1. temperaturewas heated
2. temperatureunder reflux for 15 hours
3. concentrationThe mixture was concentrated under reduced pressure
4. additionan aqueous saturated sodium bicarbonate solution was added to the mixture
5. extractionfollowed by extraction of the solution with chloroform 5 times
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (eluent: chloroform/methanol =25/1)