反应详情

Methyl pyropheophorbide-a (2, 250 mg) was dissolved in distilled tetrahydrofuran (50 ml) and 4N HCl (125 ml) was added in one lot. The reaction mixture stirred under nitrogen atmosphere at room temperature for 4 hours. The reaction was monitored by analytical tlc (silica plates), using 10% methanol/dichloromethane as a mobile phase. The reaction mixture was then poured in ice water, extracted with dichloromethane. The dichloromethane layer was washed several times with water (3×200 ml). The organic layer was separated and dried over anhydrous sodium sulfate. Evaporation of the solvent gave a residue, which was crystallized from dichloromethane/hexane. Yield, 225 mg. The purity of the compound was ascertained by tlc and the structure was confirmed by NMR spectroscopy. The NMR data were similar as described for 2 except the resonances for the —OCH3 protons of the propionic ester (—CH2CH2CO2CH3) were missing.

1. extractionextracted with dichloromethane
2. washThe dichloromethane layer was washed several times with water (3×200 ml)
3. customThe organic layer was separated
4. dry with materialdried over anhydrous sodium sulfate
5. customEvaporation of the solvent
6. customgave a residue, which
7. customwas crystallized from dichloromethane/hexane
8. customYield