反应详情

A solution of 2-(3-oxomorpholino)ethyl 2-chloroacetate (400 g, 1.81 mol) in methanol (2 L) was added dropwise to a cooled (15° C.) solution of potassium hydroxide (203 g, 3.62 mol) in methanol (10 L). This was followed by the addition methanol (3 L). The resulting solution was allowed to react overnight while the temperature was maintained at room temperature. The mixture was then filtered, and the filtrate was concentrated under reduced pressure. The resulting residue taken up in 1 L of dichloromethane, washed with 250 ml of water, dried over sodium sulfate, filtered and concentrated under reduced pressure. Purification was performed by distillation under reduced pressure (0.08 mm Hg) collecting the fraction that came over at 140° C. to afford the title compound.

1. customto react overnight while the temperature
2. filtrationThe mixture was then filtered
3. concentrationthe filtrate was concentrated under reduced pressure
4. washwashed with 250 ml of water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customPurification
9. distillationwas performed by distillation under reduced pressure (0.08 mm Hg)
10. customcollecting the fraction that
11. customcame over at 140° C.