2,6-Lutidine → HCID 86723540, compound

Participants

Reaction Steps

Trifluoromethanesulfonic anhydride (253 μL, 1.50 mmol) was added to an ice-cooled solution of 1,3-dimethyl-5-m-tolyl-8,9-dihydropyrimido[4,5-a]indolizine-2,4,10(1H,3H,7H)-trione (step 3) (388 mg, 1.15 mmol) and 2,6-lutidine (201 μL, 1.73 mmol) in DCM (7 mL). The solution was allowed to reach room temperature slowly and was stirred for 16 hours. A further portion of trifluoromethanesulfonic anhydride (39 μL, 0.23 mmol) was added and the solution was stirred for a further 30 minutes. The reaction mixture was diluted with dichloromethane (15 mL) and washed with water (2×8 mL) and sat brine (1×8 mL). The organic phase was dried with magnesium sulfate and the solvent was removed under vacuum, keeping the rotary evaporator water bath at 20° C. to give the title compound.

Provenance & Evidence