Hydrochloric Acid → HCID 136414067, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 8-bromo-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene (4.0 g, 10.3 mmol), KOH (1.73 g, 30.9 mmol), Pd2(dba)3 (189 mg, 0.2 mmol) and Xphos (350 mg, 0.82 mmol) in dioxane (20 mL) and H2O (10 mL) was purged with argon and heated at 90° C. for 45 min. The cooled reaction mixture was diluted with EtOAc and H2O then acidified with 1M HCl. The resulting precipitate was collected by filtration. The filtrate was separated, the aqueous phase extracted with further EtOAc and the combined organic extracts dried (MgSO4) and concentrated in vacuo. The resulting solid was combined with the original precipitate and triturated with Et2O. The resulting solid was collected by filtration and dried in vacuo affording 2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol as a white solid (3.01 g, 90%). LCMS: RT 2.36 min [M+H]+ 326.2

Provenance & Evidence