Claims
- 1. A process for preparing a cis-diamminediiodoplatinum(II) complex of high purity and in high yield from potassium tetraiodoplatinum(II) by a method comprising adding an aqueous solution of ammonium hydroxide to an aqueous dispersion of potassium tetraiodoplatinum(II), said tetraiodo compound having the formula K.sub.2 PtI.sub.4, under a controlled gradually rising temperature profile while controlling the ammonium hydroxide addition so that the pH does not exceed about 7.5, washing and drying the resultant precipitated cis-Pt(NH.sub.3).sub.2 I.sub.2, slowly adding the washed and dried cis-Pt(NH.sub.3).sub.2 I.sub.2 to an aqueous solution of AgNO.sub.3 at room temperature and with rapid stirring, warming the silver-containing mixture to a maximum temperature of about 50.degree. C. and maintaining the temperature of about 50.degree. C. for a period of time sufficient substantially to complete the reaction, then cooling the resultant silver-containing reaction mixture to room temperature to form a solution containing cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2 and a AgI precipitate and separating the precipitated AgI from the solution containing cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2.
- 2. A process according to claim 1, wherein the AgNO.sub.3 reagent is used in an amount slightly below stoichiometric for complete conversion of cis-Pt(NH.sub.3).sub.2 I.sub.2, and after separation of the AgI, to the remaining solution is added MCl (where M=K or Na) in a small but effective amount for precipitating Ag.sup.+, and precipitated AgCl is separated from the solution, thereby forming a purified solution of cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2 with minimized Ag.sup.+ content.
- 3. A process according to claim 1, wherein the Ag.sup.+ in solution containing cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2 is monitored with a silver/silver chloride electrode to minimize the Ag.sup.+ in solution.
- 4. A process for preparing cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2 of high purity and in high yield comprising: slowly adding a concentrated aqueous solution of KCl to a solution of chloroplatinic acid at a temperature of about 50.degree. to about 60.degree. C., to precipitate K.sub.2 PtCl.sub.6, cooling the solution to about 0.degree. C. and permitting it to stand to ensure complete precipitation, separating and washing the K.sub.2 PtCl.sub.6 precipitate, adding dropwise and at room temperature to an aqueous dispersion of the washed K.sub.2 PtCl.sub.6 an aqueous solution of N.sub.2 H.sub.4.2HCl in excess of the stoichiometric amount, warming the resultant mixture to about 60.degree. C. until the dispersed K.sub.2 PtCl.sub.6 has dissolved, thereafter heating the solution stepwise up to about 85.degree. C. thereby forming K.sub.2 PtCl.sub.4 in solution, adding an aqueous solution of KI to the aqueous solution of K.sub.2 PtCl.sub.4 to convert said K.sub.2 PtCl.sub.4 to the corresponding K.sub.2 PtCl.sub.4 at a temperature of about 40.degree. C. and maintaining the solution at a temperature to about 40.degree. C. to about 85.degree. C. to maximize conversion to K.sub.2 PtI.sub.4 to a water dispersion of said K.sub.2 PtI.sub.4, at a temperature of about 40.degree. C. adding a dilute solution of NH.sub.4 OH slowly with stirring and with pH control so that the pH of 7.5 is not exceeded during the addition until the K.sub.2 PtI.sub.4 dispersion dissolves, maintaining the resultant solution at a temperature of about 40.degree. C. to about 60.degree. C. and adding additional NH.sub.4 OH to a pH of about 7.5, then cooling the pH-adjusted solution to room temperature to precipitate cis-Pt(NH.sub.3).sub.2 I.sub.2, separating and washing the precipitated cis-Pt(NH.sub.3).sub.2 I.sub.2, adding the washed cis-Pt(NH.sub.3).sub.2 I.sub.2 to an aqueous solution of AgNO.sub.3 while stirring and at room temperature, said AgNO.sub.3 being present in a controlled amount to react with the cis-Pt(NH.sub.3).sub.2 I.sub.2 with minimum unreacted Ag, warming the silver-containing mixture to about 50.degree. C. to ensure complete reaction and then cooling the resultant silver-containing mixture thereby forming a AgI precipitate and an aqueous solution containing cis-[Pt(NH.sub.3).sub.2 (H.sub.2 O).sub.2 ](NO.sub.3).sub.2.
Parent Case Info
This is a division of application Ser. No. 241,946, filed Mar. 9, 1981, now U.S. Pat. No. 4,332,780 which in turn is a continuation-in-part of application Ser. No. 65,553, filed Aug. 16, 1979, now U.S. Pat. No. 4,273,755.
US Referenced Citations (3)
Non-Patent Literature Citations (4)
Entry |
Dhara, "A Rapid Method for the Synthesis of cis-[Pt(NH.sub.3).sub.2 Cl.sub.2 ]," Indian J. Chem., vol. 8, Feb. 1970, pp. 193, 194. |
King, "Researches on Amines Part IX", J. Chem. Soc., pt. 2, (1938), pp. 1338-1346. |
C. Lock et al, "The Structure of Platinum Anticancer Agents and Their Metabolites", J. Clin. Hematol. Oncol., 7(1), pp. 63-78, (1977). |
Chem. Abst., vol. 86, No. 24, 182241k, (1977). |
Divisions (1)
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241946 |
Mar 1981 |
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Continuation in Parts (1)
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65553 |
Aug 1979 |
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