Water → HCID 23079686, compound

Participants

Reaction Steps

4-Benzyl-2-(3-pyrrolidin-1-yl-propyl)morpholine (180 mg, 0.62 mmol) prepared according to Process Step 1 was dissolved in 1,2-dichloroethane (5 mL), and the solution was mixed with triethylamine (0.086 mL, 0.62 mmol) and 1-chloroethyl chloroformate (0.20 mL, 1.87 mmol), followed by stirring under reflux for three hours. The reaction mixture was cooled and was mixed with 1,2-dichloroethane (50 mL) and water (50 mL), followed by separation. The organic layer was washed with brine (50 mL), was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was dissolved in methanol (5 mL), followed by stirring under reflux for one hour. After distilling off the solvent under reduced pressure, diethyl ether (5 mL) was added for crystallization, and the precipitated crystals were collected by filtration. The crystals were dried under reduced pressure and thereby yielded 2-(3-pyrrolidin-1-ylpropyl)morpholine hydrochloride (135 mg, in a yield of 93%).

Provenance & Evidence