反应详情

温度

50 °C

The 1,3-bis(benzyloxy)acetone (30 g, 111 mmol) obtained in the step (4a) was mixed with ethylene glycol (64 ml, 1.148 mmol) and triethyl orthoformate (19 ml, 114 mmol), and p-toluenesulfonic acid monohydrate (591 mg, 3.11 mmol). The mixture was stirred at 50° C. for 14 hours. To the mixture, a saturated aqueous solution of sodium hydrogen carbonate and ethyl acetate were added. The organic layer was washed with water and a saline solution, dried over anhydrous sodium sulfate, and concentrated. The obtained crude product was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate=1/0-4/1 gradient) and desired fractions were concentrated to obtain the title compound (28.46 g, yield: 81.6%) as a colorless oil.

1. washThe organic layer was washed with water
2. dry with materiala saline solution, dried over anhydrous sodium sulfate
3. concentrationconcentrated
4. customThe obtained crude product
5. customwas purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate=1/0-4/1 gradient)
6. concentrationdesired fractions were concentrated