Dabco → HCID 24813637, compound

Participants

Reaction Conditions

Reaction Steps

A solution of NiCl2(dppe) (0.22 g, 0.42 mmol) in N,N-dimethylformamide (10 ml) was treated with diphenylphosphine (1.5 ml, 8.4 mmol) at 23° C. The resulting dark red solution was stirred at 120° C. for 30 min. Then a solution of trifluoromethanesulfonic acid 7-methoxy-1-[4-((R)-1-phenyl-ethylamino)-phthalazin-1-yl]-naphthalen-2-yl ester (2.3 g, 4.2 mmol) and 1,4-diazabicyclo[2.2.2]octane (DABCO, 1.9 g, 17 mmol) in N,N-dimethylformamide (13 ml) was added via a syringe, the flask was washed with N,N-dimethylformamide (2 ml). The resulting green solution was stirred at 120° C. for 17 hrs. The mixture was concentrated under reduced pressure (20 mbar, 70° C. bath temperature). The residue was purified by flash chromatography on silica gel (toluene→toluene/EtOAc 5:1) to give 1.5 g (2.5 mmol) of the title compound as an off-white solid as a 1.7:1 (1st diastereomer: 2nd diastereomer) mixture of diastereomers.

Provenance & Evidence