Step I. Synthesis of 2,2-dimethyl-1,3-dioxolan-4-one
Concentrated sulfuric acid (1 mL) was added to a solution of ethanoic acid (6.77 g, 89 mmol) in anhydrous acetone (40 mL) at 5 C and the mixture was stirred for 30 min at this temperature. It was then added to crushed ice and neutralized with sodium bicarbonate powder and extracted with dichloromethane (100 mL). The organic layer was dried with anhydrous sodium sulfate and the solvent was removed under reduced pressure to give 3.2 g 1 in 48% yield as a pure oily compound.
Step II. Synthesis of 2-morpholin-4-yl-2-one ethanol
A mixture of 2,2-dimethyl-1,3-dioxolan-4-one (116 mg, 1 mmol) and morpholine (87 mg, 1 mmol) in dichloromethane (5 mL) was stirred in argon at ambient temperature overnight and the solvent was evaporated under reduced pressure. The residue was crystallized from ethyl acetate to give 44 mg of 2-morpholin-4-yl-2-one ethanol.
