Acetate → HCID 53322417, compound

Participants

Reaction Steps

To a mixture of phosphoric acid (3b, 50 mg, 0.135 mmol) and methanol-water (3:2) was added a solution of magnesium acetate (15 mg, 0.0675 mmol. 0.5 equiv) in water (1 ml). The mixture became opaque immediately upon addition of the metal acetate and was stirred for 3 days while further precipitation occurred. The solution was concentrated to a white residue and water-methanol was added (1.4 ml). The precipitate was collected and dried; grey solid, m.p. 210° C. dec. very insoluble in water, soluble in DMSO; 1H-NMR (DMSO-d6, 300 MHz) δ 13.69 (s, 1H), 8.73 (s, 1H), 6.99 (s, 1H), 6.43 (s, 1H), 6.14 (m, 1H), 6.05 (s, 2H), 5.82 (bs, 1H), 4.41-4.31 (m, 2H), 4.03-3.95 (m, 2H). Each of the divalent cation salts proved to be only sparingly soluble in water.

Provenance & Evidence