反应详情

温度

30 °C

2,3:5,6-Di-O-isopropylidene-L-gulonolactone (22.89 g, 88.7 mmol) was dissolved in acetic acid/water (7:1, 200 ml) and stirred at 30° C. for 16 h when t.l.c. (ethyl acetate/hexane 1:1) revealed no starting material (Rf 0.5) and one major product (Rf 0.1). The solvent was removed under reduced pressure to give a yellow oil. Trituration with benzene (50 ml) gave a solid which was shaken with ethyl acetate/acetone (1:1, 250 ml). The resulting suspension was filtered and solvents removed under reduced pressure to yield an amorphous yellow solid, which was recrystallized from ethyl acetate to yield 2,3-O-isopropylidene-L-gulonolactone, (14.31 g, 79%) as a white crystalline solid, m.p. 139°-141° C., [α]D20 +76.2° (C, 1 in acetone).

1. customThe solvent was removed under reduced pressure
2. customto give a yellow oil
3. filtrationThe resulting suspension was filtered
4. customsolvents removed under reduced pressure
5. customto yield an amorphous yellow solid, which
6. customwas recrystallized from ethyl acetate