HRID1458300
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生成物
PROCEDURE
实验过程
To a suspension of lithium aluminum hydride (0.27 g) in tetrahydrofuran anhydride (40 ml) was added a solution of N-(1,2-diethyl-4-pyrazolidinyl)-4-geranyloxybenzamide (0.89 g) in tetrahydrofuran anhydride (10 ml) dropwise while being cooled with ice. After being refluxed with heating for 5 hours, the reaction solution, with aqueous solution of sodium potassium tartrate added thereto, was extracted with dichloromethane. The extract was concentrated under a vacuum and thus obtained residue was purified by silica gel column chromatography (chloroform:methanol=40:1), thereby yielding 0.31 g (36%) of the aimed compound.
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后处理
- temperaturewhile being cooled with ice
- temperatureAfter being refluxed
- temperaturewith heating for 5 hours
- extractionwas extracted with dichloromethane
- concentrationThe extract was concentrated under a vacuum and thus obtained residue
- customwas purified by silica gel column chromatography (chloroform:methanol=40:1)