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In water; at 20℃; for 1h; |
A 0.4M solution of tetrabutylammonium hydroxide in H2O (2.89 mL,1.156 mmoles) was added drop by drop and under stirring to a suspension of <strong>[638-53-9]<strong>[638-53-9]tridecanoic</strong> acid</strong> (0.278 g, 1.277 mmoles) in MiIIiQ H2O (20 mL). The resulting suspension was left under stirring at room temperature for 1 hour, the solid was removed by filtration and the filtrate was then used without further treatment.The reactions were carried out shielded from light, under nitrogen <n="26"/>atmosphere and in MiIIiQ H2O. AgNO3 (0.0655 g, 0.386 mmoles) was added to a solution of {mu-(l,8, l l, 18-tetraazaoctadecane-N',N18)bis[tr<ms- diamino(dichloro)platinum(II)] tetranitrate (0.2 g, 0.193 mmoles) in H2O (23 mL) and the resulting suspension was left under stirring at room temperature for 24 hours. The solid was removed filtering the mixture twice over a double microfiber filter; the filter was washed with 1 ml H2O which was pooled with the filtrate. The filtrate was added drop by drop and under stirring with the above prepared solution of tetrabutylammonium tridecanoate; the resulting solution was kept under stirring at room temperature overnight. The separated sticky material was collected, washed with H2O, dried under vacuum at 3O0C and suspended in hexane (12 mL); the mixture was left under stirring overnight and the resulting solid was collected on a buchner filter, washed with hexane and dried under vacuum at 300C to give 0.098 g (25% yield) of a clear powder.Elemental Calculated C 55.28% H 9.99% nu 5.61% Pt 19.52% AnalysisFound C 54.42% H 9.82% N 5.45% Pt 19.06%MS: 1355.3, [MHH-C3F7COOH^CI 2H25COOH]+ 1H NMR (CD3OD): delta 2.89 (4H, s); 2.73 (4H, t, J=7.59 Hz); 2.61 (4H, t, J=7.70); 2.19 (12H, m); 1.60 (2OH, m); 1.41 (8H, m); 1.29 (108H, m); 0.90 (18H, t, J=6.83). |
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In water; at 20℃; for 1h; |
Example 4{mu-(1,8,11,18-Tetraazaoctadecane-N1,N18)bis[trans-diamino(tridecanoato-O)platinum(II)]tetratridecanoate A 0.4M solution of tetrabutylammonium hydroxide in H2O (2.89 mL, 1.156 mmoles) was added drop by drop and under stirring to a suspension of <strong>[638-53-9]<strong>[638-53-9]tridecanoic</strong> acid</strong> (0.278 g, 1.277 mmoles) in MilliQ H2O (20 mL). The resulting suspension was left under stirring at room temperature for 1 hour, the solid was removed by filtration and the filtrate was then used without further treatment.The reactions were carried out shielded from light, under nitrogen atmosphere and in MilliQ H2O. AgNO3 (0.0655 g, 0.386 mmoles) was added to a solution of {mu-(1,8,11,18-tetraazaoctadecane-N1,N18)bis[trans-diamino(dichloro)platinum(II)]tetranitrate (0.2 g, 0.193 mmoles) in H2O (23 mL) and the resulting suspension was left under stirring at room temperature for 24 hours. The solid was removed filtering the mixture twice over a double microfiber filter; the filter was washed with 1 ml H2O which was pooled with the filtrate. The filtrate was added drop by drop and under stirring with the above prepared solution of tetrabutylammonium tridecanoate; the resulting solution was kept under stirring at room temperature overnight. The separated sticky material was collected, washed with H2O, dried under vacuum at 30 C. and suspended in hexane (12 mL); the mixture was left under stirring overnight and the resulting solid was collected on a buchner filter, washed with hexane and dried under vacuum at 30 C. to give 0.098 g (25% yield) of a clear powder. Elemental Calculated C 55.28% H 9.99% N 5.61% Pt 19.52% Analysis Found C 54.42% H 9.82% N 5.45% Pt 19.06% MS: 1355.3, [MH+C3F7COOH-4C12H25COOH]+ 1H NMR (CD3OD): delta 2.89 (4H, s); 2.73 (4H, t, J=7.59 Hz); 2.61 (4H, t, J=7.70); 2.19 (12H, m); 1.60 (20H, m); 1.41 (8H, m); 1.29 (108H, m); 0.90 (18H, t, J=6.83). |
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