Potassium Phosphate, Tribasic → HCID 58243435, compound

Participants

Reaction Steps

1-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (21 mg, 101 μmol), tricyclohexylphosphine (3.1 mg, 11 μmol) and Pd2(dba)3 (4.2 mg, 5 μmol) were dissolved in dioxane (0.25 ml) under a nitrogen atmosphere. Solid 1-cyclobutyl-4-{[3-(4-iodophenoxy)azetidin-1-yl]carbonyl}-1,4-diazepane (42 mg, 92 μmol) was added followed by K3PO4 (122 μl of a 1.27 M aqueous solution, 156 μmol). The reaction was stirred at room temperature for 30 minutes and then at 110° C. for 16 hours. The reaction was diluted with dichloromethane (30 ml), filtered through celite, washed twice with saturated NaHCO3 (15 ml), dried (MgSO4), filtered and concentrated at reduced pressure. The residue was purified by FCC (DCM/MeOH/NH3 with gradient, 98:2:1 to 90:10:1) and then recrystallised (Heptane/EtOAc) to give the title product as white solid (16 mg, 42%).

Provenance & Evidence