反应详情

Potassium hydroxide (274.27 g) and HO(CH2)3OH (371.93 g) were added to dioxane (3 L), and then TsOCH(CH3)CH2OC(CH3)3 (700 g) prepared in Example 2-1 was added gradually. The reaction solution was refluxed with heating for 16 hours, allowed to cool, and poured onto ice (500 g), neutralized with 2 N hydrochloric acid, concentrated and filtered to remove the precipitated salt. The filtrate was extracted with dichloromethane (250 mL), and the organic layer was washed with water (500 mL) repeatedly 17 times. The organic layer was dried over magnesium sulfate and filtered, and the filtrate was concentrated with an evaporator, and the concentrate was purified by silica gel chromatography to give the title compound (203.77 g). The NMR spectrum data of the product were as follows.

1. temperatureThe reaction solution was refluxed
2. temperaturewith heating for 16 hours
3. temperatureto cool
4. additionpoured onto ice (500 g)
5. concentrationconcentrated
6. filtrationfiltered
7. customto remove the precipitated salt
8. extractionThe filtrate was extracted with dichloromethane (250 mL)
9. washthe organic layer was washed with water (500 mL) repeatedly 17 times
10. dry with materialThe organic layer was dried over magnesium sulfate
11. filtrationfiltered
12. concentrationthe filtrate was concentrated with an evaporator
13. customthe concentrate was purified by silica gel chromatography