Dichloromethane → (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate

Temperatur

42.5 °C

Hexahydrofuro[2,3-b]furan-3-yl acetate (124 g) to the RB flask along with buffer solution (118 g Sodium dihydrogen phosphate dihydrate dissolved in 600 ml water & pH adjusted to 6.5 with saturated NaHCO3 aqueous solution). CAL-B enzyme (19.5 g) was added to the reaction mass and stirred at 40-45° C. Reaction was monitored by Chiral-GC. Reaction was cooled to room temp., dichloromethane (1300 ml) was charged to reaction mass and filtered through hyflow bed. Dichloromethane layer was separated and washed with Sodium chloride solution (10%, 650 ml) and water (3×650 ml). Dichloromethane layer was concentrated under vacuum to get residue of (3R,3aS,6aR)-Hexahydrofuro[2,3-b]furan-3-yl acetate (Yield 53 g). Further, the product was purified by fractional distillation under vacuum at 98-118° C. to get main fraction 39.5 g having purity 97.98%.

1. additionCAL-B enzyme (19.5 g) was added to the reaction mass
2. customReaction
3. customReaction
4. temperaturewas cooled to room temp.
5. filtrationfiltered through hyflow bed
6. customDichloromethane layer was separated
7. washwashed with Sodium chloride solution (10%, 650 ml) and water (3×650 ml)
8. concentrationDichloromethane layer was concentrated under vacuum

ORD-Eintrag

ord-6834833e4545493db374aef79cde797e

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08841467B2