Acetone → (R)-isopropylidenebutane-1,2,4-triol

(R)-(+)-1,2,4-Butanetriol (0.7 g, 6.6 mmol), prepared as described in step a) above, was stirred for 1.5 h in acetone (50 ml) containing 3 drops of conc. perchloric acid, a satured solution of sodium bicarbonate in water (5 ml) was added and the stirring was continued for additional 10 min. The precipitate was filtered off and the filtrate evaporated under reduced pressure (2.7 kPa, 30° C.). The residue was taken up in ethyl acetate, washed with saturated aqueous sodium bicarbonate (5 ml) and brine (5 ml), and dried over magnesium sulphate. Evaporation of the solvent and distillation gave the title compound as a colourless oil (0.3 g, 2.05 mmol, 31%): b.p. 104°-106° C. at~2.7 kPa. nD20 =1.4390.

1. filtrationThe precipitate was filtered off
2. customthe filtrate evaporated under reduced pressure (2.7 kPa, 30° C.)
3. washwashed with saturated aqueous sodium bicarbonate (5 ml) and brine (5 ml)
4. dry with materialdried over magnesium sulphate
5. customEvaporation of the solvent and distillation

ORD-Eintrag

ord-95dc4a34650b47ee84da867cb13429a5

Quelldatensatz

uspto-grants-1991_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05036071