preparation | step 1. 2,2-dimethyl -1,3-dioxolane -4-one synthesis of concentrated sulfuric acid (1mL) is added to the anhydrous acetone (40mL) solution of glycolic acid (6.77g,89mmol) at 5 ℃, and stir the mixture at this temperature for 30 minutes. 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 obtain 3.2g 1 in 48% yield, which is a pure oily compound. Step 2. the synthesis of 2-morpholin-4-yl-2-one ethanol The 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 overnight in argon at ambient temperature, and the solvent was evaporated under reduced pressure. The residue crystallized from ethyl acetate to give 44mg of 2-morpholin-4-yl-2-one ethanol. |