Acetone → Diacetone-D-glucose

Temperatur

60 °C

To 200 ml of acetone were added 10.0 g of D-glucose and 100 mg of hydrogen iodide and the mixture was refluxed with stirring in a water bath at 60° C. for 8 hours. During this reaction, the refluxing solvent was dried with 20 g of Molecular Sieves 3A interposed between the reaction vessel and the cooling jacket. After completion of the reaction, a small amount of pyridine was added. The acetone was then distilled off under reduced pressure and the residue was dissolved in benzene, washed with aqueous sodium bicarbonate and water and dried over anhydrous magnesium sulfate. The benzene was distilled off under reduced pressure to give 11.5 g (80.0%) of 1,2:5,6-di-O-isopropylidene-α-D-glucofuranose. After recrystallization from chloroform-hexane (1:2), it melted at 107°-109° C.

1. temperaturethe mixture was refluxed
2. customDuring this reaction
3. dry with materialthe refluxing solvent was dried with 20 g of Molecular Sieves 3A
4. customAfter completion of the reaction
5. distillationThe acetone was then distilled off under reduced pressure
6. dissolutionthe residue was dissolved in benzene
7. washwashed with aqueous sodium bicarbonate and water
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationThe benzene was distilled off under reduced pressure

ORD-Eintrag

ord-6eda1e8c119c4ad88b58cba32bd75600

Quelldatensatz

uspto-grants-1984_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04464530