反应详情

To a solution of N,N'-Bis[2,3-bis(acetyloxy)propyl]-5-(4)-(R)-(hydroxymethyl)-2-oxo-3-oxazolidinyl]-2,4,6-triiodo-1,3-benzenedicarboxamide of Example 2b (0.410 g, 0.51 mmol) in anhydrous methanol (7 ml) was added a methanolic solution of sodium methoxide (1.18 ml, 1M solution) and the mixture was stirred at room temperature for 1 h. The methanol was then removed on the rotary evaporator and water (8 ml) was added to redissolve the white residue. Dowex-50 (H+) was added to this solution portionwise to bring the pH down to approximately 7.0. The Dowex-50 resin was filtered off, water was removed on the rotary evaporator, and the white solid dried in vacuo at 60° over P2O5. The solid thus obtained (0.350 g) was redissolved in water (0.5 ml), seeded with a tiny crystal of the racemate and left overnight. The crystallized product was filtered, washed with cold water and dried overnight over P2O5 to obtain N,N'-Bis[2,3-bis(acetyloxy)propyl]-5-(4)-(R)-(hydroxymethyl)-2-oxo-3-oxazolidinyl]-2,4,6-triiodo-1,3-benzenedicarboxamide as white crystalline needles (0.32 g, 84%).

1. customThe methanol was then removed on the rotary evaporator and water (8 ml)
2. additionwas added
3. dissolutionto redissolve the white residue
4. additionDowex-50 (H+) was added to this solution portionwise
5. filtrationThe Dowex-50 resin was filtered off
6. customwater was removed on the rotary evaporator
7. dry with materialthe white solid dried in vacuo at 60° over P2O5
8. customThe solid thus obtained (0.350 g)
9. waitleft overnight
10. filtrationThe crystallized product was filtered
11. washwashed with cold water
12. dry with materialdried overnight over P2O5