Crystalline form of 2-((1′-n-hexyloxy) ethyl)-2-divinyl-pyropheophorbide-a and method for preparing thereof

摘要

The present invention provides a crystalline form of HPPH (2-((1′-n-hexyloxy)ethyl)-2-divinyl-pyropheophorbide-a):;
The crystalline form can be characterized by an X-ray powder diffraction (XRD) pattern and differential scanning calorimeter (DSC) pattern. The present invention also provides a method for preparing the crystalline form of HPPH.

主权项

1. A method for preparing the crystalline form of 2-((1′-n-hexyloxy) ethyl)-2-divinyl-pyropheophorbide-a (HPPH) characterized by at least one of the features set forth below:
(1) characteristic peaks (2θ) of X-ray powder diffraction (XRD) pattern being: (2θ±0.2) 5.46°, 6.02°, 13.95°, 18.03°, 24.01°, 24.49°; (2) characteristic peak of differential scanning calorimeter (DSC) pattern: a characteristic endothermic peak being at 201.2° C., comprising the four steps set forth below: 1) dissolving an HPPH sample into a polar organic solvent; 2) adding a non-polar solvent to promote crystallization of the HPPH; 3) mixing the mixture, then continuously stirring or sitting undisturbed for 1 to 8 hrs; 4) isolating the obtained crystal, wherein, the polar solvent is selected from ethyl acetate or acetone, the non-polar solvent is selected from n-hexane or n-heptane, and the step of isolating comprises filtering and drying.