反应详情

Ethyl 2-ethoxy-6-pentadecyl-benzoate (10.9 g, 27 mmol) was dissolved in dry tetrahydrofuran (60 mL). This solution was transferred to dry 250 mL three neck round bottom flask fitted with reflux condenser, mechanical stirrer and it was maintained under nitrogen atmosphere through out the reaction. To this lithium aluminum hydride (2.04 g, 54 mmol) was added slowly. Reaction was highly exothermic. After addition the solution was slowly brought to the reflux temperature and maintained at that temperature for about two hours and TLC was checked in hexane:EtOAc (8:2). After completion of reaction, excess lithium aluminum hydride was decomposed by drop-wise addition of ethylacetate (80 mL). To this 5 M HCl (100 mL) was added and organic layer was separated, dried over anhydrous sodium sulphate, concentrated under vacuum to give a light brownish solid. This was recrystallised from petroleum ether (40-60° C.) to give white solid. Yield: 8 g.

1. dry with materialto dry 250 mL three neck round bottom flask
2. customfitted
3. temperaturewith reflux condenser, mechanical stirrer
4. temperatureit was maintained under nitrogen atmosphere through out the reaction
5. customReaction
6. additionAfter addition the solution
7. temperaturemaintained at that temperature for about two hours
8. customorganic layer was separated
9. dry with materialdried over anhydrous sodium sulphate
10. concentrationconcentrated under vacuum
11. customto give a light brownish solid
12. customThis was recrystallised from petroleum ether (40-60° C.)
13. customto give white solid