Диссертация (1150306), страница 14
Текст из файла (страница 14)
G&+,F*. &4%5*1+%4& 4%'% 6 (200 414*'() F )%,.*4#,&)# (1 4', 5'2 6) %'% F 4#,&)*'# (1 4', 5'2 4) 5*9&F'2'% 1.&+,F*.: 1*4"'#1+& 30 %'% 31 (100 414*'() F )%,.*4#,&)# (2 4'). X*4*/#))HJ .&+,F*.*+,&F'2'% )& 10 0 ".% 1*4)&,)*J ,#4"#.&,:.# (30) %'% )& 100 0 ".% –8 ºC (31). ?9.&I*F&FS%#+2*+&51% *,K%'(,.*FHF&'%, ".*4HF&'% )%,.*4#,&)*4 (2 "*.$%% "* 2 4') % +:S%'% F ,#0#)%# 12 0".% 1*4)&,)*J ,#4"#.&,:.# )& F*I5:3#.!!77!(Cl)2HMeONNOFH+*1*/*NHHN73%.B.&I' 225 °C.;H0%+'#)*5'2-&J5#)*: C, 21.46; H, 4.55; N, 19.75%.
Z!>-O!+HPt;H3*5C10H24N8Cl2O2Pt•aH2O: C, 21.32; H, 4.47; N, 19.89.NHNMe2N[44](Cl)2NMe2Me.&I.#S#)%2(MeOH,m/z):482.155([Md 2Cl d H]+, FH0%+'#)* 482.154). >C (KBr, *,5#'()H#"*'*+H, +4d1): 3432(+.), 3425(+.), 3290(+.), 3181(+.),3058(+.) b(NdH); 2925(+'), 2853(+'), 2824(+') b(CdH);H1649(+%'), 1613(+.) b(C=N); 767(+'), 724(+'), 687(+') f(CdH). AOG 1H (Me2SO-56, f): 8.60 (+, 1H,NH2), 8.00 (+, 1H, NH2), 7.11 (+, :S%., 1H, NH), 3.09 (+, :S%., 6H, NMe2), 2.73 (+, 3H, CH3).(Cl)2HPhONPtNN82%.B.&I' 168 °C.;H0%+'#)*5'2C, 35.08; H, 4.36; N, 16.26%. Z!>-O!+ FH+*1*/* .&I.#S#)%2O(MeOH, m/z): 303.593 ([M d 2Cl]2+, FH0%+'#)* 303.596),NHH;H3*5C20H28N8Cl2O2Pt•aH2O: C, 34.94; H, 4.25; N, 16.30. -&J5#)*:NHHNMe2N[45](Cl)2.NMe2Ph606.177 ([M d 2Cl d H]+, FH0%+'#)* 606.185).
>C (KBr,*,5#'()H# "*'*+H, +4d1): 3448(+.), 3414(+%'), 3401(+%'),3151(+.) b(NdH); 2990(+.), 2959(+.), 2926(+.) b(CdH);H1649(+%') b(C=N); 778(+'), 694(+') f(CdH). AOG 1H (Me2SO-56, f): 9.10 (+, 1H, NH2), 8.84 (+, 1H,NH2), 7.85–7.60 (4, 6H, NH+Ar), 2.73 (+, :S%., 6H, NMe2). C.%+,&''H, ".%/*5)H# 5'2 G!7,9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F ^,&)*'# )& F*I5:3# ".%1*4)&,)*J ,#4"#.&,:.#.HNHONNPt[49](Cl)2.;H3*562%.B.&I' 156 °C.;H0%+'#)*5'2C10H24N8Cl2O2Pt•2H2O: C, 20.34; H, 4.78; N, 18.98.
-&J5#)*: C,NNHMe2N(Cl)2HMe Me20.46; H, 4.67; N, 18.87%. Z!>-O!+ FH+*1*/* .&I.#S#)%2HO(MeOH, m/z): 482.149 ([M d 2Cl d H]+, FH0%+'#)* 482.154). >CNHNMe2(KBr, *,5#'()H# "*'*+H, +4d1): 3406(+%'), 3246(+.), 3150(+.)b(NdH); 2935(+') b(CdH); 1643(+%') b(C=N); 726(+'), 682(+') f(CdH). AOG 1H (Me2SO-56, f):8.70 (+, 1H, NH2), 8.55 (+, 1H, NH2), 8.01 (+, :S%., 1H, NH), 3.11 (+, :S%., 6H, NMe2), 2.17 (+, 3H,CH3).HPh PhNHOMe2N(Cl)2HNNNPtNHNHH[50](Cl)2.;H3*575%.B.&I' 142 °C.;H0%+'#)*5'2C20H28N8Cl2O2Pt•2H2O: C, 33.62; H, 4.51; N, 15.68. -&J5#)*: C,33.43; H, 4.67; N, 15.68%.
Z!>-O!+ FH+*1*/* .&I.#S#)%2(MeOH, m/z): 303.597 ([M d 2Cl]2+, FH0%+'#)* 303.596). >CONMe2(KBr, *,5#'()H# "*'*+H, +4d1): 3448(+%') b(NdH); 2961(+'),2932(+'), 2875(+') b(CdH); 1636(+%') b(C=N); 776(+'), 690(+')f(CdH). AOG 1H (Me2SO-56, f): 8.87 (+, :S%., 1H, NH), 8.25 (+, :S%., 1H, NH2), 7.94 (+, :S%.,!78!!1H, NH2), 7.67d7.60 (4, 3H, o- % #-CH), 7.49 (,, 2H, 3-CH), 3.15 (+, 6H, NMe2). C.%+,&''H,".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F)%,.*4#,&)# )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.(9<D=7> <P7GED87PEF 4, 6 8 %&"'!/()!-[PtCl2(RCN)2] (R = Et, Ph) 26–29.
!4#+(&4%5*1+%4& 4 %'% 6 (220 414*'() % 1*4"'#1+& 26–29 (100 414*'() .&+,F*.2'% (".% "*':0#)%%57 % 59) %'% +:+"#)I%.*F&'% (".% "*':0#)%% 56, 58, 60 % 61) F )%,.*4#,&)# (3 4'). >),#)+%F)*"#.#4#S%F&2 +:+"#)I%2 (%'% /*4*/#))HJ .&+,F*. 9#I "#.#4#S%F&)%2) *+,&F'2'% )& 24 0 (28% 29) %'% )& 48 0 (26 % 27) ".% 1*4)&,)*J ,#4"#.&,:.#, "*+'# 0#/* .#&1$%*))&2 +4#+(*3'&Y5&'% 5* 4 ºC. ?9.&I*F&FS%#+2 +F#,'*-YU',H# "*.*S1% *,K%'(,.*F&'%, ".*4H'% CHCl3 (2"*.$%% "* 1 4') % +:S%'% F ,#0#)%# 12 0 ".% 1*4)&,)*J ,#4"#.&,:.# )& F*I5:3#.PhHHNONMeMeClNHPtHNClC18H22N6Cl2O2Pt•aH2O: C, 34.35; H, 3.68; N, 13.35.NO56. ;H3*5 83%.
B.&I' 156 °C. ;H0%+'#)* 5'2NHHFH+*1*/*Ph+-&J5#)*: C, 34.36; H, 3.66; N, 13.19%. Z!>-O!+.&I.#S#)%2(MeOH,m/z):548.125+([M d 2Cl d H] , FH0%+'#)* 548.132), 585.100 ([M – Cl] , FH0%+'#)* 585.109), 621.073 ([M + H]+,FH0%+'#)* 621.085), 643.056 ([M + Na]+, FH0%+'#)* 643.067), 1168.198 ([2M d 2Cl d H]+,FH0%+'#)* 1168.210), 1205.173 ([2M – Cl]+, FH0%+'#)* 1205.187), 1258.179 ([2M + NH4]+,FH0%+'#)* 1258.190), 1789.230 ([3M – 2Cl d H]+, FH0%+'#)* 1789.288), 1861.219 ([3M + H]+,FH0%+'#)* 1861.241), 1883.195 ([3M + Na]+, FH0%+'#)* 1883.223).
>C (KBr, *,5#'()H# "*'*+H,+4d1): 3494(+.), 3354(+.-+%'), 3188(+.-+%') b(NdH); 3056(+'), 3003(+'), 2968(+'), 2925(+')b(CdH); 1669(+.-+%'), 1623(*0 +%') b(C=N); 778(+.), 702(+'), 690(+.) f(CdH). B!R (^'T#),:3'*.*K*.4:&$#,*) = 4:1, 2/0.5 4') Rf = 0.35. AOG 1H (Me2SO-56, f): 8.32 (5, 2H, o-CH), 8.18 (+,:S%., 1H, NH), 7.69 (,, 1H, #-CH), 7.57 (,, 2H, 3-CH), 7.10 (+, :S%., 1H, NH), 6.84 (+, :S%., 1H,NH), 1.91 (+, 3H, CH3).PhHHNPhClONNH57. ;H3*5 87%. B.&I' 143 °C. ;H0%+'#)* 5'2PhPtHNClPhC28H26N6Cl2O2Pt•H2O: C, 44.10; H, 3.70; N, 11.02.NONHH-&J5#)*: C, 44.08; H, 3.52; N, 11.13%.
Z!>-O!+FH+*1*/* .&I.#S#)%2 (MeOH:Me2SO = 10:1, m/z):787.157 ([M – Cl + Me2SO]+, FH0%+'#)* 787.154).>C (KBr, *,5#'()H# "*'*+H, +4d1): 3491(+.-+%'), 3340(+.-+%'), 3283(+.-+%'), 3258("') b(NdH);3173 (+'), 3055(+') b(CdH); 1622(*0 +%') b(C=N); 777(+.-+%'), 696(+%') f(CdH). B!R (^'T#),:3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.66.
AOG 1H (Me2SO-56, f): 8.90 (5, 2H, o-CH), 8.47 (+,:S%., 1H, NH), 7.85 (5, 2H, o-CH), 7.72 (,, 1H, #-CH), 7.63–7.50 (4, 5H, 3-, #-CH), 7.39 (+, :S%.,2H, NH2).!!79!ClEtEtPtNOH58. ;H3*5 66%. B.&I' 154 °C. ;H0%+'#)* 5'2 C10H22N6Cl2O2Pt: C,ClNHN22.91; H, 4.23; N, 16.03. -&J5#)*: C, 22.78; H, 4.19; N, 16.14%.Z!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 452.133 ([M –OH2Cl – H]+, FH0%+'#)* 452.132), 489.111 ([M – Cl]+, FH0%+'#)*HN489.109), 525.093 ([M + H]+, FH0%+'#)* 525.085), 542.147NNHHMeMe([M + NH4]+, FH0%+'#)* 542.112).
>C (KBr, *,5#'()H# "*'*+H,+4d1): 3496(+.), 3344(+%'), 3201(+.) b(NdH); 3083(+.), 2941(+'-c.), 2881(+') b(CdH); 1664(+.-+%'),1626(*0 +%') b(C=N); 794(+'), 700(+'-c.) f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 1:1, 1/1 4')Rf = 0.62. AOG 1H (Me2SO-56, f): 7.92 (+, :S%., 1H, NH), 6.90 (+, :S%., 1H, NH), 6.62 (+, :S%.,1H, NH), 2.89 (1, 2H, CH2), 1.81 (+, 3H, CH3), 1.25 (,, 3H, CH3).ClEtClNOHOHB.&I' 149 °C.;H0%+'#)*5'2(MeOH, m/z): 576.167 ([M – 2Cl – H]+, FH0%+'#)* 576.163),NHPhPh69%.36.28; H, 4.17; N, 12.65%. Z!>-O!+ FH+*1*/* .&I.#S#)%2HNNH;H3*5C20H26N6Cl2O2Pt•"H2O: C, 36.29; H, 4.19; N, 12.70. -&J5#)*: C,NHN59.EtPt613.143 ([M – Cl]+, FH0%+'#)* 613.140), 649.120 ([M + H]+,FH0%+'#)* 649.117), 666.149 ([M + NH4]+, FH0%+'#)* 666.143),687.077 ([M + K]+, FH0%+'#)* 687.073), 1261.260 ([2M – Cl]+, FH0%+'#)* 1261.249), 1314.263([2M + NH4]+, FH0%+'#)* 1314.253), 1335.203 ([2M + K]+, FH0%+'#)* 1335.182).
>C (KBr,*,5#'()H# "*'*+H, +4d1): 3496(+.), 3373(+.), 3299(+%'), 3227(+.-+%'), 3185(+.) b(NdH); 3059(+'c.), 2988(+'-c.), 2941(+'-c.), 2918(+'), 2888(+'), 2849(+') b(CdH); 1671(+%'), 1629(*0 +%')b(C=N); 777(+'), 695(+') f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 4:1, 2/0.5 4') Rf = 0.57.AOG 1H (Me2SO-56, f): 8.38 (+, :S%., 1H, NH), 7.85 (5, 2H, o-CH), 7.55–7.40 (4, 3H, 3-, #-CH),7.16 (+, :S%., 2H, NH2), 3.00 (1, 2H, CH2), 1.35 (,, 3H, CH3). C.%+,&''H, ".%/*5)H# 5'2 G!7,9H'% FH.&M#)H %I .#&1$%*))*J +4#+% F )%,.*4#,&)# ".% 1*4)&,)*J ,#4"#.&,:.#.ClPhPhPtNH60. ;H3*5 81%.
B.&I' 152 °C. ;H0%+'#)* 5'2 C18H22N6Cl2O2Pt: C,ClONHNHZ!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 621.090 ([M + H]+,ONFH0%+'#)* 621.085), 643.073 ([M + Na]+, FH0%+'#)* 643.067),H659.046 ([M + K]+, FH0%+'#)* 659.041), 1241.175 ([2M + H]+,NNH34.85; H, 3.57; N, 13.55. -&J5#)*: C, 34.91; H, 3.49; N, 13.47%.MeMeHFH0%+'#)*1241.163),1263.160([2M + Na]+,FH0%+'#)*1263.145), 1279.135 ([2M + K]+, FH0%+'#)* 1279.119).
>C (KBr, *,5#'()H# "*'*+H, +4d1):3495(+.-+%'), 3448(+.), 3376(+.-+%'), 3321(+%'), 3219(+.-+%'), 3187(+.-+%') b(NdH); 3062(+'),2980(+'), 2932(+') b(CdH); 1658(+%'), 1622(*0 +%') b(C=N); 785(+.), 699(+') f(CdH). B!R(^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.44. AOG 1H (Me2SO-56, f): 8.61 (5, 2H, o-CH),!80!!7.79 (+, :S%., 1H, NH), 7.70–7.50 (4, 3H, 3-, #-CH), 6.96 (+, :S%., 1H, NH), 6.64 (+, :S%., 1H,NH), 1.75 (+, 3H, CH3).ClPhClPtNOH45.17; H, 3.52; N, 11.29.
-&J5#)*: C, 45.01; H, 3.49; N, 11.42%.NHN61. ;H3*5 87%. B.&I' 153 °C. ;H0%+'#)* 5'2 C28H26N6Cl2O2Pt: C,PhHZ!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 709.147 ([M – Cl]+,OHNFH0%+'#)* 709.140), 745.123 ([M + H]+, FH0%+'#)* 745.117),NNHHPhPh767.107 ([M + Na]+, FH0%+'#)* 767.096), 783.080 ([M + K]+,FH0%+'#)* 783.073), 1453.262 ([2M – Cl]+, FH0%+'#)* 1453.249),1489.234 ([2M + H]+, FH0%+'#)* 1489.226), 1511.221 ([2M + Na]+, FH0%+'#)* 1511.208), 1527.197([2M + K]+, FH0%+'#)* 1527.182). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3482(+.), 3363(+.-+%'),3288(+.-+%') b(NdH); 3059(+'), 2922(+'), 2859(+') b(CdH); 1636(+%'), 1612(*0 +%'), b(C=N);776(+.), 694(+.) f(CdH).