2-Chloroethanol → HCID 67996924, compound

Participants

Reaction Conditions

Reaction Steps

About 200 mL of acetonitrile (manufactured by Junsei Co., Ltd. in Japan) was mixed with about 52.7 mL (0.5 mol) of methylpyrrolidone (manufactured by Fluka Co., Ltd.) under a nitrogen atmosphere to form a liquid mixture. Subsequently, about 36.5 mL (0.55 mol) of 2-chloroethanol (manufactured by Aldrich Co., Ltd.) was added to the liquid mixture drop by drop to form a mixed solution. Subsequently, the mixed solution was stirred at about 65° C. for about 48 hours under a nitrogen atmosphere, and was then stored at about 4° C. for about 12 hours to form crystals. After a supernatant was removed from the mixed solution, the crystals were dried at a temperature of about 35° C. and a pressure of about 0.2 atm for about 12 hours using a vacuum evaporator to remove a solvent therefrom. Subsequently, in order to remove impurity, the dried crystals were dissolved in about 100 mL of acetone, and were then stirred at a temperature of about 25° C. and a pressure of about 1 atm for about 30 minutes to form a solution. The solution was stored at about 4° C. for about 12 hours to form crystals again. After a supernatant was removed from the solution, the crystals were dried at a temperature of about 35° C. and a pressure of about 0.2 atm for about 12 hours using a vacuum evaporator. These processes were repeatedly conducted three times to obtain N-hydroxyethyl-N-methylpyrrolidinium chloride at a yield of about 60%.

Provenance & Evidence