Lithium Hydroxide → HCID 70061469, compound

Participants

Reaction Steps

The lactone derivative prepared as usual by coupling of 4-[[4-(aminoiminomethyl)phenyl]amino]-4-oxobutanoic acid hydrochloride prepared in Example 1, Step 1 and 3-amino-4hydroxyfuran was dissolved in water (20 mL) and the pH adjusted to 10.5 by addition of LiOH H2O. The reaction was allowed to proceed at room temperature for 2 hours and the product isolated by RPHPLC. The appropriate fractions were adjusted to pH 7 by addition of LiOH prior to solvent removal. Subsequent lyophilization gave a white solid: 1H NMR (d6DMSO) δ 2.5 (m, 6H), 2.9 (m, 1H), 4.08 (m, 1H ), 4.42 (m, 2H ), 7.80 (s, 4H), 8.5 (d, 1H), 8.85 (s, 2H), 9.15 (s, 2H), 10.4 (s, 1H). MS (FAB) 337.1 (MH+), 319.2 (M-H2O+H). Elemental analysis; Required for C15H20N4O5. CF3CO2H 1.5 H2O: C 42.77 H 5.07 N 11.74 Found: C 43.06 H 4.24 N 11.45

Provenance & Evidence