Hydrochloric Acid → HCID 24829229, compound

Participants

Reaction Steps

To a solution of Compound 16 (15.7 mg, 0.02 mmol) in 1,4-dioxane (1 mL) at 0-5° C. was added 4M HCl(g) in 1,4-dioxane (1 mL) dropwise over ˜15 min. The resulting mixture was allowed to warm to room temperature. Ether (˜15 mL) was added to the reaction mixture and stirred for 10 min. The resulting mixture was placed in the freezer for 1 h. The solid residue was filtered and washed with ether and quickly dissolved in 18μΩ deionized water. Evaporation of the aqueous solution gave pure Compound 17 (12.4 mg, 90%) as an orange solid. 1H NMR (CD3OD) δ 2.82-3.48 (m, 13H), 3.78-4.08 (m, 10H), 6.76 (d, 1H), 7.40-7.55 (m, 4H), 8.51 (d, 1H). HRMS (Positive ion FAB) Calcd for C27H34N8O9 [M+H]+ m/z 615.2527. Found: [M+H]+ m/z 615.2520. Analytical HPLC (tR=3.6 min, Method 2).

Provenance & Evidence