反应详情

温度

4 °C

A solution of lithium aluminum hydride (1.0 g, 26 mmol) in tetrahydrofuran (50 mL) was cooled to 4° C., and a solution of methyl 3,5-bis(methoxymethoxy)phenylacetate (5.3 g, 20 mmol) obtained in Example 1, Step 1 in tetrahydrofuran (50 mL) was added dropwise thereto, followed by stirring at 4° C. for 30 minutes. To the reaction mixture was added anhydrous sodium sulfate decahydrate to stop the reaction, and the mixture was stirred at room temperature for 12 hours. The resulting suspension was filtered under reduced pressure, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/9-1/1) to obtain 2-[3,5-bis(methoxymethoxy)phenyl]ethanol (4.6 g, 98%). 1H-NMR (CDCl3, 270 MHz) δ (ppm): 6.62 (t, J=2.2 Hz, 1H), 6.58 (d, J=2.2 Hz, 2H), 5.14 (s, 4H), 3.85 (q, J=6.4 Hz, 2H), 3.48 (s, 6H), 2.81 (t, J=6.4 Hz, 2H), 1.42 (t, J=6.4 Hz, 1H)

1. customthe reaction
2. stirringthe mixture was stirred at room temperature for 12 hours
3. filtrationThe resulting suspension was filtered under reduced pressure
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/9-1/1)