Sodium Hydroxide → HCID 86671459, compound

Participants

Reaction Steps

To chlorosulfonic acid (4 mL) at 0° C. was added 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene (400 mg, 1.35 mmol) portion wise and the resulting mixture stirred for 5 min then added drop wise to ice. NaOH (7.2 g) in H2O (20 mL) was added to the mixture and stirred for 1 h at RT then concentrated in vacuo. The resulting residue was purified by column chromatography (C18, gradient 0.5-1% MeOH in H2O) then extracted into hot MeOH. Upon cooling the mixture was filtered and the filtrate concentrated in vacuo affording Sodium 2-(2-isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene-9-sulfonate (1.32 g) contaminated with inorganic salts. LCMS: RT 2.14 min [M+H]+ 376.1

Provenance & Evidence