Crystallization CIMS

Deacetylisocolchicine-DF-amide. A solution of the DADF derivative (40 mg, 0.05 mmol) in methanol (2ml) was added with 4 drops of concentrated ammonium hydroxide, and the solution was stirred at room temperature for 0.5 hr. The solvent was evaporated and the residue crystallized from CH2C12 to afford orange crystals (30 mg, 90%) mp 220°C [a]D-198° (0.1, MeOH) CIMS 674 (M+) UV (EtOH) 210 and 344 nm, (EtOH + NaOH) 237 and 346 nm. 

Figure 23.25. Plots of integrated WAXD intensity as a function of 26 for (a) CIM and (b) OSIM samples. The numbers on the left sides represent the distance away from the sample surface ( i,m). The (130)o, and (117). reflections at 26 = 18.6° and 20.1°, respectively, typical of the a- and 7-crystal of iPP, are also indicated...

The fraction of 7-crystal, f, with respect to a-crystal in samples, was calculated and the distribution of through the depth of samples was shown in Figure 23.26. FVom the distribution curves of f, it can be seen that the spatial distribution of 7-crystal is different for CIM and OSIM samples. The of CIM samples increased monotonously in outer... 

Figure 23.26. Fraction of 7-crystal with respect to a-crystal, evaluated from the X-ray diffraction profiles from skin to core region of CIM and OSIM samples...

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