反应详情

A mixture of N-benzhydryl-2,5-anhydro-2,5-imino-D-glucitol (Formula XI, R3 =Ph2CH 8.40 g, 25.5 mmol) and 0.42 g of 20% PD(OH)2 /carbon in 100 mL of MeOH was set shaking on a Parr apparatus under 60 psig of hydrogen overnight. This solution was then filtered and concentrated. Hexane (ca. 300 mi) was added, and the solvent was then removed from a white solid, which was washed with ca. 200 mL of hexane. The product was recrystallized from ETOH/CH3CN to give 3.79 g (91%) of white needles, mp 139°-142.50° C. (corrected). Both 1H and 13C NMR in D2O supported the assigned structure.

1. filtrationThis solution was then filtered
2. concentrationconcentrated
3. additionHexane (ca. 300 mi) was added
4. customthe solvent was then removed from a white solid, which
5. washwas washed with ca. 200 mL of hexane
6. customThe product was recrystallized from ETOH/CH3CN