Sodium Methoxide → HCID 136051363, compound

Participants

Reaction Steps

To a solution of 15 (1.25 g, 1.94 mmol) in dry methanol (100 mL) was added sodium methoxide powder until the pH reached 10. The solution was stirred overnight and then neutralized with Dowex H+ resin and filtered. After evaporation of the filtrate, the residue was washed with ether to remove methyl benzoate and the crude material was crystallized from water: yield 520 mg, 81%: mp 220° C. dec.: UV λmax 1H NMR (DMSO-d6) δ6.48 (d, J=3.00 Hz, 1H, C1, H), 6.99 (s, 2H, NH2), 11.47 (s, 1H, NH), and other sugar protons. Anal. Calcd. for C10H12N4O5S2.H2O: C, z34.28: H, 4.03: N, 15.99: S, 18.30. Found: C, 33.99: H, 3.92: N, 15.68: S, 18.22.

Provenance & Evidence