Acetic Anhydride → Hexahydrofuro[2,3-b]furan-3-yl acetate

Temperatur

5 °C

Hexahydrofuro[2,3-b]furan-3-ol (25 g) was dissolved in dichloromethane (250 ml) and added triethylamine (23.3 g). N,N-dimethylaminopyridine (0.46 g) was added to the reaction mass. Reaction mass was cooled to 0-10° C. Acetic anhydride (21.5 g) was diluted with dichloromethane (50 ml) & added slowly drop-wise to the reaction mass. Reaction mass was stirred at 0-5° C. till completion. Reaction mass was washed with water (2×100 ml) & 10% Sodium chloride solution (100 ml). Reaction mass was concentrated under vacuum at <40° C. to get residue of Hexahydrofuro[2,3-b]furan-3-yl acetate (yield 29 g). Further, the product was purified by distillation (20 g) under vacuum using fractional distillation at 88-102° C. to get main fraction 17 g having purity 92.6%

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2. additionadded slowly
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5. washwas washed with water (2×100 ml) & 10% Sodium chloride solution (100 ml)
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7. concentrationwas concentrated under vacuum at <40° C.

ORD-Eintrag

ord-a7dd7ca8078f4adcb4feb2a925d82b30

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08841467B2