HCID 178435494, compound → HCID 178435492, compound

Participants

Reaction Steps

To a solution of methyl pheophorbide-a (100 g, 165 mmol) in 2,6-lutidine (4 L) was added distilled water (40 mL, 2.22 mol, 13 equiv., 1% v/v) and the mixture was refluxed under argon with stirring. The reaction was monitored by HPLC (hexane-acetone, 90:10-mobile phase, LiChrospherCN-column, detection at 425 and 410 nm). The HPLC of reaction aliquot after 90 min showed 99.5% of completion. The solution was cooled to room temperature after 120 min of reflux and solvent removed under reduced pressure with water bath at 45-50° C. Hexane (120 mL) was added and the solid was collected by filtration and rinsed with hexane to remove any traces of 2,6-lutidine. The solid was vacuum dried to give methyl pyropheophorbide-a (89.6 g, 99%).

Provenance & Evidence