| 78% |
Stage #1: bis{trans(diammine)(chloro)platinum (II)}-μ-(1,16-diamino-7,10-diazahexadecane-N1,N16) dinitrate With silver nitrate In water at 20℃; for 24h;
Stage #2: sodium caproate In methanol; water at 20℃; for 24h;
Stage #3: sodium dodecyl-sulfate In water at 20℃; for 0.25h; |
13
The reactions were carried out shielded from light and in MiIIiQ H2O. A solution of { μ-(l,8, l l , 18-tetraazaoctadecane-N1,N18)bis[?r««5- diamino(dichloro)platinum(II)] } tetranitrate (0.2 g, 0.193 mmoles) in H2O (18 mL) was added with AgNO3 (0.072 g, 0.424 mmoles) and the resulting suspension was kept under stirring for 24 hrs. The solid was removed filtering the mixture twice on a double microfibre filter and the filter was washed with 1 mL of H2O which was pooled with the filtrate. The filtrate was added drop by drop and under stirring with a sodium capronate solution (0.16 g, 1.158 mmoles) in MeOH (19 mL); the resulting solution was maintained under stirring at room temperature for 24 hrs, then concentrated to half volume (350C) under reduced pressure and added drop by drop and under stirring with a sodium dodecylsulphate solution (0.222 g, 0.77 mmoles) in H2O (15 mL). After stirring for 15 min at room temperature, the precipitated solid was collected on a buchner filter, washed with few millilitres of water and dried under vacuum at 35°C to give 0.301 g (78% yield) of the title product.Elemental Calculated C H 8 .52% N 5 .57% Pt SAnalysis 44 .21 % 19 .40% 6. 38%Found C H 8 .42% N 5 .45% Pt S43 .53 % 19 .02% 6. 80%1H NMR (CD3OD): δ 4.17 (12H, bs); 4.00 (8H, t, J = 6.58 Hz); 3.20 (4H, s); 2.98 (4H, t, J = 7.5); 2.65 (4H, m); 2.18 (4H, t, J = 8.24); 1.76-1.21 (108H, m); 0.90 (18H, m). |
| 78% |
Stage #1: bis{trans(diammine)(chloro)platinum (II)}-μ-(1,16-diamino-7,10-diazahexadecane-N1,N16) dinitrate With silver nitrate In water at 20℃; for 24h; Darkness;
Stage #2: sodium caproate In methanol; water at 20℃; for 24h;
Stage #3: sodium dodecyl-sulfate In methanol; water at 20℃; for 0.25h; |
13
Example 13; {μ-(1,8,11,18-Tetraazaoctadecane-N1,N18)bis[trans-diamino(capronato-O)platinum(II)]tetra(dodecylsulphate) The reactions were carried out shielded from light and in MilliQ H2O. A solution of {μ-(1,8,11,18-tetraazaoctadecane-N1,N18)bis[trans-diamino(dichloro)platinum(II)]tetranitrate (0.2 g, 0.193 mmoles) in H2O (18 mL) was added with AgNO3 (0.072 g, 0.424 mmoles) and the resulting suspension was kept under stirring for 24 hrs. The solid was removed filtering the mixture twice on a double microfibre filter and the filter was washed with 1 mL of H2O which was pooled with the filtrate. The filtrate was added drop by drop and under stirring with a sodium capronate solution (0.16 g, 1.158 mmoles) in MeOH (19 mL); the resulting solution was maintained under stirring at room temperature for 24 hrs, then concentrated to half volume (35° C.) under reduced pressure and added drop by drop and under stirring with a sodium dodecylsulphate solution (0.222 g, 0.77 mmoles) in H2O (15 mL). After stirring for 15 min at room temperature, the precipitated solid was collected on a buchner filter, washed with few millilitres of water and dried under vacuum at 35° C. to give 0.301 g (78% yield) of the title product. Elemental Calculated C 44.21% H 8.52% N 5.57% Pt 19.40% S 6.38% Analysis Found C 43.53% H 8.42% N 5.45% Pt 19.02% S 6.80% 1H NMR (CD3OD): δ 4.17 (12H, bs); 4.00 (8H, t, J=6.58 Hz); 3.20 (4H, s); 2.98 (4H, t, J=7.5); 2.65 (4H, m); 2.18 (4H, t, J=8.24); 1.76-1.21 (108H, m); 0.90 (18H, m). |
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