Dimethylformamide → HCID 69519861, compound

Participants

Reaction Steps

A mixture of Example 8 (9 mg, 0.018 mmol), tetrakis(triphenylphosphine)-palladium (22 mg, 0.019 mmol), and Zn(CN)2 (15 mg, 0.128 mmol) in DMF (1 mL) stirring under argon was heated to 120° for 1 h. After cooling to RT, the heterogeneous was diluted with a 80% MeOH in H2O solution and filtered. The filtrate was directly injected to reverse phase preparative HPLC, which provided the title compound (7 mg). HPLC/MS retention time=3.3 min (Phenomenex Luna 5 micron C18 4.6 mm×50 mm column eluted with a 0% to 100% B solvent gradient over 4 min; solvent A=90% H2O, 10% MeOH, 10 mM NH4OAc and solvent B=10% H2O, 90% MeOH, 10 mM NH4OAc; flow rate=4.0 mL/min; UV detection at 220 nm); m/z=418 [M+H]+, 416 [M−H]−.

Provenance & Evidence