Hydrochloric Acid → 2-Heptylpropane-1,3-diol

In anhydrous diethyl ether was dissolved 100 g of the obtained diethyl heptylmalonate, and the mixture was added dropwise to a solution of 28.7 g of lithium aluminum hydride dispersed in 270 ml of diethyl ether. The mixture was stirred for 15 hours. Then, to the reaction mixture was added gradually 3N hydrochloric acid to make excess lithium aluminum hydride inactive. After washing with 10% aqueous solution of sodium carbonate, then water, the resulting ether layer dried with anhydrous magnesium sulfate. After distilling ether under reduced pressure, the residue was purified by silica gel chromatography (developing solvent: hexane/ethyl acetate=4/1) and distilled under reduced pressure to give 41.2 of 2-heptyl-1,3-propanediol (yield: 6%).

1. washAfter washing with 10% aqueous solution of sodium carbonate
2. dry with materialwater, the resulting ether layer dried with anhydrous magnesium sulfate
3. distillationAfter distilling ether under reduced pressure
4. customthe residue was purified by silica gel chromatography (developing solvent: hexane/ethyl acetate=4/1)
5. distillationdistilled under reduced pressure

ORDレコード

ord-8c2fb60c2d7645ebbc0128cdb821aa63

出典データセット

uspto-grants-1991_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05053507