反应详情

The substrate (20) (1.1 g) was dissolved in CH3OH/NH3 at 0° C. and placed in a steel bomb. The bomb was closed and stirred at room temperature for 18 h. The steel bomb was cooled, opened and evaporated to dryness. The residue was tried to crystallization with little ethanol. The product crystallized, but on filtration, the crystals re-absorbed water and became a paste. The crystallization repeated several times. Finally it crystallized from Methanol/Ethanol mixture. The colorless crystals was filtered, washed with methanol and dried in vacuo. The filtrate was evaporated again which on standing gave further crystals. Total yield 0.5 g (72%); mp: 177-179° C.; [a]D=+38.33 (c 3 mg/mL H2O); D form of Ribavirin [a]D=−36.0 (c 3.0 mg/mL H2O); 1H NMR (Me2SO-d6) δ3.46 (m, 1H, C5′H), 3.60 (m, 1H, C5′H), 3.92 (q, 1H, C4′H), 4.12 (q, 1H), 4.34 (q, 1H), 4.88 (t, 1H, C5′OH), 5.20 (d, 1H), 5.58 (d, 1H), 5.80 (d, 1H, C1′H), 7.60 (bs, 1H, NH), 7.82 (bs, 1H, NH), and 8.82 (s, 1H, C3H). Anal. Calc. for C8H12N4O5 (244.20): C, 39.34; H, 4.95; N, 22.94. Found: C, 39.23; H, 4.97; N, 22.91.

1. customThe bomb was closed
2. customevaporated to dryness
3. customThe residue was tried to crystallization with little ethanol
4. customThe product crystallized
5. filtrationon filtration
6. customthe crystals re-absorbed water
7. customThe crystallization
8. customFinally it crystallized from Methanol/Ethanol mixture
9. filtrationThe colorless crystals was filtered
10. washwashed with methanol
11. customdried in vacuo
12. customThe filtrate was evaporated again which on standing
13. customgave further crystals