Synthetic and Purification Methods for Phosphaplatin Compounds and Uses Thereof
a technology of phosphaplatin and purification method, which is applied in the field of synthetic methods for the preparation of phosphaplatin compounds, can solve problems such as literature limitations, and achieve the effects of reducing time, reducing the limitation on the upper end of concentration, and reducing the tim
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example 1
Synthesis of trans-(1R,2R)-DACH-Pt—Cl2
[0101]Potassium tetrachloroplatinate (85.0 gm 0.02 mole) was dissolved in 633 ml of deionized water and filtered. To the resulting red solution was added a solution of trans-(1R,2R)-cyclohexyldiamine (28.0 gm 0.24 mole) dissolved in 126 ml of deionized water. The resulting reaction mixture was stirred for 66 hours at 20° C. during which time a yellow precipitate formed. The suspension was filtered and the solids washed sequentially with deionized water (500 ml) and methanol (402 gm), followed by vacuum drying at 40° C. / 25 mbar, to afford 71.11 gm (91.3%) yield of a yellow solid, trans-(1R,2R)-DACH-Pt—Cl2. HPLC purity; 98.8% area.
example 2
Synthesis of (R,R)-DACH-2 (Repeating Bose Method at an 8× Scale)
[0102]Trans-(1R,2R)-DACH-Pt—Cl2 (0.8 gm, 1.649 mmole) was added to a solution of tetrasodium pyrophosphate decahydrate (3.2 gm, 7.10 mmole) in 1981 ml of deionized water. The solution was adjusted to pH 8 with 2 N nitric acid (approx. 0.08 gm), heated to 40° C. and stirred for 15 hours during which time the pH decreased to about 6.6. The reaction mixture was concentrated to a residual volume of 40 ml by reduced pressure evaporation. The pH of the concentrate was 5.7. The stirred solution, immersed in an ice bath, was adjusted to pH 2 with 2 N nitric acid (approx. 1 gm). A precipitate slowly formed which was isolated by filtration and washed sequentially with cold deionized water (79 ml) and acetone (63 gm). Vacuum drying afforded a greenish solid. The first experiment afforded 0.13 gm (6.3%), while the second afforded 0.30 gm (29.8%) product. The latter sample showed a single 31P NMR resonance at +1.51 ppm (bicarbonate ...
example 3
Portion-wise Addition of DACH-Pt—Cl2
[0103]Tetrasodium pyrophosphate decahydrate (20.5 gm 46 mmole) was dissolved in 250 ml of deionized water. The mixture was adjusted to pH 8 with 2 N nitric acid (3-5 ml). The solution was heated to 40° C. and DACH-Pt—Cl2 (5.0 gm, 13.1 mmole) was added in 5×1 gm portions over an 8 hr period. The resulting suspension was stirred for an additional 15 hr at 40° C. during which time all of the solids did not dissolve. The reaction mixture was increased to 60° C. and stirring was continued for an additional 22 hour during which time all of the solids had dissolved to afford a clear greenish colored solution. The solution was cooled to ambient temperature and the pH adjusted to 2 with 2 N nitric acid (30-35 ml). On further cooling to 5° C. a precipitate formed. The green solid was collected by filtration, and sequentially washed with deionized water (3×15 ml) and methanol (3×15 ml). Vacuum drying afforded 2.6 gm (40.9% yield) of a greenish colored solid...
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