Carbon tetrabromide → HCID 136383562, compound

Participants

Reaction Steps

Triphenylphosphine (0.168, 0.64 mmol) was added to a mixture of 4-[1-(3-hydroxy-propyl)-5-fluoro-indol-3-yl]-5-(1-H-indol-3-yl)-2,4-dihydro-[1,2,4]triazol-3-one (0.23 g 0.59 mmol), synthesised in accordance to the procedure for Example 1, triphenylphosphine (0.168 g, 0.64 mmol) and tetrabromomethane (0.218 g, 0.66 mmol) in dry THF (15 ml). The resulting mixture was stirred at ambient temperature. After 16 h the LCMS showed that some starting material still was left. Additional tetrabromomethane (0.198 g, 0,60 mmol) and triphenylphosphine (0.158 g, 0.60 mmol) were added and the solution was allowed to proceed for 20 h more at ambient temperature. Evaporation and silica gel chromatography (dichloromethane/methanol, gradient to 100/5) afforded 0.165 g (57%) of the title compound as a white solid.

Provenance & Evidence