Sodium Acetate → HCID 178476932, compound

Participants

Reaction Steps

To a solution of diethyl ester 12b (2.73 g, 4 mmol) in ethanol (60 mL) was treated with sodium ethanoate in ethanol (6 mmol, 6 mL of 1 M solution) under a nitrogen atmosphere. The mixture was stirred for 18 h at room temperature, and then acidified with Amberlite IR-120 (H+-form). The heterogeneous solution was stirred at 40° C. for 3 h, filtered and concentrated in vacuo. The residual oil was taken up in water (15 mL) and subjected to lyophilization. The residual colorless solids were washed with cold acetone (20 mL×3), dissolved in aqueous NH4HCO3 (15 mL of 0.1 M solution), stirred for 1 h at room temperature, and then lyophilization to afford ammonium salt 13c of Tamiphosphor guanidine monoester (1.22 g, 75%) as white solids.

Provenance & Evidence