Диссертация (1150306), страница 16
Текст из файла (страница 16)
>C (KBr, *,5#'()H# "*'*+H, +4–1): 3410 (+%'),Me3368 (+%') b(N–H); 3033 (*0 +'), 2992 (*0 +'), 2966 (*0 +')b(C–H); 2288 (+.) b(C!N); 1666 (+.-+%'), 1623 (+.-+%') b(C=N). AOG 1H (Me2SO-56, f): 8.91 (+,:S%., 1H, NH2), 8.55 (+, :S%., 1H, NH2), 7.60 (+, :S%., 1H, NH), 7.42 (5, 2H, CH), 7.20 (5, 2H,CH), 3.15–2.98 (4, 8H, NCH2), 2.33 (+, 3H, CH3), 1.62–1.48 (4, 6H, CH2), 1.22–1.03 (4, 6H, CH2).HNClPtNC5H10NNClNC5H10[72](Cl).;H3*567%.;H0%+'#)*5'2C19H28N6OCl2Pt•2H2O: C, 34.66; H, 4.90; N, 12.76.-&J5#)*: C, 34.81; H, 4.81; N, 12.64%.
Z!>-O!+OFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 479.092 ([M –NCNC5H10 – Cl]+,H2NFH0%+'#)*479.085).>C(KBr,*,5#'()H# "*'*+H, +4–1): 3416 (+%'), 3358 (+p) b(N–H);3045 (*0 +'), 2932 (+') b(C–H); 2295(+.-+%') b(C!N); 1666 (+.-+%'), 1626 (+.-+%') b(C=N).AOG 1H (Me2SO-56, f): 8.86 (+, :S%., 1H, NH2), 8.54 (+, :S%., 1H, NH2), 7.75–7.72 (4, 4H,NH + )-, #-!!), 7.61 (,, 2H, 3-CH), 3.41–3.19 (4, 8H, NCH2), 1.60–1.48 (4, 6H, CH2), 1.23–1.03 (4,6H, CH2).HNClPtNNClNC5H10[73](Cl).;H3*580%.;H0%+'#)*5'2C20H27N7OCl2Pt•2H2O: C, 35.14; H, 4.57; N, 14.34.-&J5#)*: C, 35.12; H, 4.59; N, 14.47%. Z!>-O!+OFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 502.073 ([M –C5H10NH2NCN!!86!NCNC5H10 – Cl]+, FH0%+'#)* 502.072), 612.157 ([M – Cl]+, FH0%+'#)* 612.156).
>C (KBr,*,5#'()H# "*'*+H, +4–1): 3410 (+%'), 3368 (+%') b(N–H); 3038 (*0 +'), 2992 (*0 +'), 2966 (*0 +')b(C–H); 2268(+.) % 2228(+%') b(C!N); 1666 (+.-+%'), 1623 (+.-+%') b(C=N). AOG 1H (Me2SO-56,f): 8.93 (+, :S%., 1H, NH2), 8.64 (+, :S%., 1H, NH2), 7.70 (+, :S%., 1H, NH), 7.65 (5, 2H, CH), 7.32(5, 2H, CH), 3.24–2.95 (4, 8H, NCH2), 1.66–1.50 (4, 6H, CH2), 1.30–1.07 (4, 6H, CH2).HNClPtNC5H10NNNC5H10Cl[74](Cl).;H3*584%.;H0%+'#)*5'2C19H27N7O3Cl2Pt•2H2O: C, 32.44; H, 4.44; N, 13.94.-&J5#)*: C, 32.38; H, 4.49; N, 13.93%.
Z!>-O!+OFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 522.063 ([M –H2NNCNC5H10 – Cl]+, FH0%+'#)* 522.061), 632.147 ([M – Cl]+,NO2FH0%+'#)* 623.146). >C (KBr, *,5#'()H# "*'*+H, +4–1):3415 (+%'), 3368 (+%') b(N–H); 3038 (*0 +'), 2992 (*0 +'), 2969 (*0 +') b(C–H); 2288 (+.) b(C!N);1666 (+.-+%'), 1624 (+.-+%') b(C=N); 1520(+%') b(N=O)a+; 1342(+%') b(N=O)c. AOG 1H (Me2SO-56,f): 8.95 (+, :S%., 1H, NH2), 8.64 (+, :S%., 1H, NH2), 7.72 (+, :S%., 1H, NH), 7.62 (5, 2H, CH), 7.34(5, 2H, CH), 3.19–2.98 (4, 8H, NCH2), 1.66–1.52 (4, 6H, CH2), 1.31–1.12 (4, 6H, CH2).5.5.2 !7A;9R Q:EG?D;EF FA?;:7PEH9D?H>:AESE 8E@9;<A7> <P7GAEC S:?QQB 8G7<HD7H=7<A<P7GEP 75–82 (EZV<> P9;EG7D<)C .&+,F*.: +F#Y#".%/*,*F'#))*/* 3#'&,)*/* 1*4"'#1+& 33, 68–74 F 3'*.*K*.4# (2 4'),0#.#I 7 4%) "*+'# +4#S#)%2 .#&/#),*F, ".%9&F'2'% .&+,F*.
B67 (100 414*'() F 3'*.*K*.4#(1 4'). G#&1$%*)):T +4#+( *+,&F'2'% )& 1 0 ".% 40 ºC % I&,#4 .&,F*. *3'&Y5&'% 5* 1*4)&,)*J,#4"#.&,:.H. ?9.&I*F&FS%J+2 *+&5*1 *,K%'(,.*F&'%, ".*4H'% !-!l3 (2 "*.$%% "* 0.5 4') %FH+:S%'% F ,#0#)%# 12 0 ".% 1*4)&,)*J ,#4"#.&,:.# )& F*I5:3# (".% "*':0#)%% 76–78, 81 %82). G&+,F*. 9H' )&)#+U) )& +%'%1&/#'( F 1*.*,1*J (5'%)& 7 +4, 5%&4#,. 0.7 +4) 1*'*)1# %3.*4&,*/.&K%.*F&) (^'T#),: 3'*.*K*.4/)%,.*4#,&) = 5:1, 5'2 75; 12 4' 3'*.*K*.4& %, I&,#4,3'*.*K*.4/)%,.*4#,&) = 3:2, 5'2 79 % 80). !*9%.&'% "#.F&2 K.&1$%T % .&+,F*.%,#'(:"&.%F&'% ".% "*)%Y#))*4 5&F'#)%% ".% 1*4)&,)*J ,#4"#.&,:.#.
C*4"'#1+H 75, 79 % 80+:S%'% F ,#0#)%# 1 0 ".% 10 49&.. 8*':0#))H# $%&)&,)H# 1*4"'#1+H 75, 79 % 80 +*5#.Y&'%)#9*'(S*# 1*'%0#+,F* (~5–10 4*'%) 5%3'*.%5)*/* 1*4"'#1+& (91, 95 % 96, +**,F#,+,F#))*) F1&0#+,F# ".%4#+%.!!87!75. ;H3*5 58%. Z!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 441.140NMe2Cl([M d NCO – Cl – H]+, FH0%+'#)* 441.136), 478.117 ([M d NCO]+,HNPtOCNFH0%+'#)* 478.112), 484.147 ([M d Cl]+, FH0%+'#)* 484.142), 521.124NH([M + H]+, FH0%+'#)* 521.118), 543.109 ([M + Na]+, FH0%+'#)* 543.100),NMe2N559.079([M + K]+,FH0%+'#)*559.074),997.223([2M d NCO]+,FH0%+'#)* 997.225), 1003.260 ([2M d Cl]+, FH0%+'#)* 1003.252),Me1062.219 ([2M + Na]+, FH0%+'#)* 1062.210), 1078.195 ([2M + K]+,FH0%+'#)* 1078.184).
Z!>-O!– FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 519.109 ([M d H]–,FH0%+'#)* 519.102), 1038.225 ([2M d H]–, FH0%+'#)* 1038.213). >C (KBr, *,5#'()H# "*'*+H,+4d1): 3448(+.), 3379(+.-+%') b(NdH); 2217(*0 +%') b(OCN); 1665(*0 +%'), 1624(+.-+%') b(C=N);1551(+%') f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.47.
AOG 1H (Me2CO-56,f): 8.84 (+, :S%., 1H, NH), 7.42 (5, 2H, CH), 7.28 (5, 2H, CH), 5.98 (++5, 2JPtH = 34 X$, :S%., 1H,NH), 3.05 (+, 6H, N(CH3)2), 2.58 (+, 6H, N(CH3)2), 2.39 (+, 3H, CH3).76. ;H3*5 74%. ;H0%+'#)* 5'2 C13H19N6OClPt•aH2O: C, 30.33; H, 3.92;NMe2ClN, 16.32. -&J5#)*: C, 30.64; H, 3.86; N, 16.10%. Z!>-O!+ FH+*1*/*HNPtOCNNH.&I.#S#)%2 (MeOH, m/z): 464.093 ([M d NCO]+, FH0%+'#)* 464.092),N470.102 ([M d Cl]+, FH0%+'#)* 470.121), 529.081 ([M + Na]+, FH0%+'#)*Me2N529.080), 545.054 ([M + K]+, FH0%+'#)* 545.054), 1034.165 ([2M + Na]+,FH0%+'#)* 1034.171), 1050.138 ([2M + K]+, FH0%+'#)* 1050.145). Z!>-O!– FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 505.086 ([M d H]–, FH0%+'#)* 505.082), 1010.197([2M d H]–, FH0%+'#)* 1010.173).
>C (KBr, *,5#'()H# "*'*+H, +4d1): 3382(+.), 3245(+.),3221(+.) b(NdH); 2250(*0 +%') b(OCN); 1666(*0 +%'), 1619(+.-+%') b(C=N); 1515(+%') f(NdH).B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.42. AOG 1H (Me2CO-56, f): 9.03 (+, :S%.,1H, NH), 7.55–7.45 (4, 5H, CH), 5.99 (++5, 2JPtH = 34 X$, :S%., 1H, NH), 3.04 (+, 6H, NMe2), 2.57(+, 6H, NMe2). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%%.&+,F*.& 1*4"'#1+& F +4#+% 4#,&)*'-)%,.*4#,&) (1:1 "* *9_#4:) )& F*I5:3# ".% 1*4)&,)*J,#4"#.&,:.#.NMe2Cl77. ;H3*5 85%.
;H0%+'#)* 5'2 C14H18N7OClPt•H2O: C, 30.63; H, 3.67;HNPtOCNN, 17.86. -&J5#)*: C, 30.58; H, 3.74; N, 17.94%. Z!>-O!+ FH+*1*/*NH.&I.#S#)%2 (MeOH, m/z): 489.094 ([M d NCO]+, FH0%+'#)* 489.088),N495.121 ([M d Cl]+, FH0%+'#)* 495.117), 554.084 ([M + Na]+, FH0%+'#)*Me2N554.075), 570.060 ([M + K]+, FH0%+'#)* 570.049). Z!>-O!– FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 530.088 ([M d H]–, FH0%+'#)* 530.078),CN1060.179 ([2M d H]–, FH0%+'#)* 1060.164).
>C (KBr, *,5#'()H# "*'*+H,+4d1): 3432(+.), 3403(+.), 3345(+.), 3278(+'-c.) b(NdH); 2245(*0 +%') b(OCN); 2232(+.-+%')!88!!b(C`N); 1664(*0 +%'), 1648(+%') b(C=N); 1539(+%') f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) =2:1, 2/1 4') Rf = 0.32. AOG 1H (Me2CO-56, f): 9.02 (+, :S%., 1H, NH), 7.88 (5, 2H, CH), 7.76 (5, 2H,CH), 5.96 (+, :S%., 1H, NH), 3.00 (+, 6H, NMe2), 2.55 (+, 6H, NMe2).78.
;H3*5 87%. ;H0%+'#)* 5'2 C13H18N7O3ClPt•aCHCl3: C, 26.56; H,NMe2Cl3.05; N, 16.06. -&J5#)*: C, 26.50; H, 3.21; N, 15.93%. Z!>-O!+HNPtOCNNHFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 472.103 ([M d NCO – Cl – H]+,NFH0%+'#)* 472.101), 509.087 ([M d NCO]+, FH0%+'#)* 509.077),Me2N515.100([M d Cl]+,FH0%+'#)*515.106),574.070([M + Na]+,FH0%+'#)* 574.065), 590.043 ([M + K]+, FH0%+'#)* 590.039). Z!>-O!–NO2FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 550.078 ([M d H]–, FH0%+'#)*550.068), 1100.159 ([2M d H]–, FH0%+'#)* 1100.143). >C (KBr, *,5#'()H# "*'*+H, +4d1):3430(+.-+%'), 3390(+.-+%'), 3230(+'-c.) b(NdH); 2231(*0 +%') b(OCN); 1666(*0 +%'), 1638(+.+%') b(C=N); 1521(+.-+%') b(N=O)a+, 1346(+%') b(N=O)c.
B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1,2/1 4') Rf = 0.34. AOG 1H (Me2CO-56, f): 9.05 (+, :S%., 1H, NH), 8.31 (5, 2H, CH), 7.82 (5, 2H,CH), 5.98 (+, :S%., 1H, NH), 3.00 (+, 6H, NMe2), 2.55 (+, 6H, NMe2). C.%+,&''H, ".%/*5)H# 5'2G!7, 9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F +4#+% 4#,&)*')%,.*4#,&) (1:1 "* *9_#4:) )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.NC5H10ClHNPtOCN79. ;H3*5 65%. Z!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 521.200([M d NCO – Cl – H]+, FH0%+'#)* 521.199), 558.176 ([M d NCO]+,NHFH0%+'#)* 558.175), 564.203 ([M d Cl]+, FH0%+'#)* 564.205), 601.182N([M + H]+, FH0%+'#)* 601.181), 623.164 ([M + Na]+, FH0%+'#)* 623.163),C5H10N639.138 ([M + K]+, FH0%+'#)* 639.136), 1157.335 ([2M d NCO]+,FH0%+'#)* 1157.348), 1163.360 ([2M d Cl]+, FH0%+'#)* 1163.377),Me1200.338 ([M + H]+, FH0%+'#)* 1200.354), 1222.319 ([2M + Na]+,FH0%+'#)* 1222.336), 1239.293 ([2M + K]+, FH0%+'#)* 1239.310).
Z!>-O!– FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 599.173 ([M d H]–, FH0%+'#)* 599.165), 1198.342 ([2M d H]–,FH0%+'#)* 1198.338). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3451(+.), 3361(+.) b(NdH); 2938(+%'),2852(+.-+%') b(CdH); 2266(*0 +%') b(OCN); 1659(*0 +%'), 1621(+%') b(C=N); 1528(+.) f(NdH).B!R (^'T#),: 3'*.*K*.4:&$#,*) = 5:1, 2.5/0.5 4') Rf = 0.51. AOG 1H (Me2CO-56, f): 9.28 (+,:S%., 1H, NH), 7.37 (5, 2H, CH), 7.29 (5, 2H, CH), 6.41 (+, :S%., 1H, NH), 3.40–3.20 (4, 8H,NCH2), 1.65–1.55 (4, 6H, CH2), 1.20–1.10 (4, 6H, CH2).!!89!NC5H10ClHNPtOCN80. ;H3*5 52%. Z!>-O!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 507.185([M d NCO – Cl – H]+,NHFH0%+'#)*507.183),544.162([M d NCO]+,FH0%+'#)* 544.159), 550.191 ([M d Cl]+, FH0%+'#)* 550.189), 609.151N([M + Na]+, FH0%+'#)* 609.147), 625.123 ([M + K]+, FH0%+'#)* 625.121),C5H10N1129.310 ([2M d NCO]+, FH0%+'#)* 1129.317), 1138.336 ([2M d Cl]+,FH0%+'#)* 1135.346), 1194.294 ([2M + Na]+, FH0%+'#)* 1194.307),1210.265 ([2M + K]+, FH0%+'#)* 1210.278).
Z!>-O!– FH+*1*/* .&I.#S#)%2 (MeOH, m/z):585.160 ([M d H]–, FH0%+'#)* 585.149), 1170.321 ([2M d H]–, FH0%+'#)* 1170.307). >C (KBr,*,5#'()H# "*'*+H, +4d1): 3448(+.), 3375(+.) b(NdH); 2932(+%'), 2853(+.-+%') b(CdH);2269(*0 +%') b(OCN); 1659(*0 +%'), 1624(+%') b(C=N); 1521(+.) f(NdH). B!R (^'T#),:3'*.*K*.4:&$#,*) = 5:1, 2.5/0.5 4') Rf = 0.53. AOG 1H (Me2CO-56, f): 9.37 (+, :S%., 1H, NH),7.49–7.45 (4, 5H, Ph), 6.44 (++5, 2JPtH = 34 X$, :S%., 1H, NH), 3.40–3.20 (4, 8H, NCH2), 1.65–1.55(4, 6H, CH2), 1.20–1.10 (4, 6H, CH2).81. ;H3*5 86%.
;H0%+'#)* 5'2 C20H26N7OClPt•aCHCl3: C, 36.71; H,NC5H10ClHNPtOCN3.98; N, 14.62. -&J5#)*: C, 36.70; H, 4.05; N, 14.62%. Z!>-O!+NHFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 532.179 ([M d NCO – Cl – H]+,NFH0%+'#)* 532.173), 569.155 ([M d NCO]+, FH0%+'#)* 569.150), 575.181C5H10N([M d Cl]+, FH0%+'#)* 575.179), 634.142 ([M + Na]+, FH0%+'#)* 634.138),650.117([M + K]+,FH0%+'#)*650.112),1243.280([2M + Na]+,FH0%+'#)* 1244.287), 1261.254 ([2M + K]+, FH0%+'#)* 1261.260).
Z!>-CNO!– FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 610.156 ([M d H]–, FH0%+'#)* 610.140), 1220.309([2M d H]–, FH0%+'#)* 1220.289). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3429(+.-+%'), 3367(+.)b(NdH);2943(+%'),2859(+.-+%')b(CdH);2270(*0 +%')b(OCN);2231(+.-+%')b(C`N);1660(*0 +%'), 1631(+.-+%') b(C=N); 1526(+.) f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 3:1,1.5/0.5 4') Rf = 0.43. AOG 1H (Me2CO-56, f): 9.60 (+, :S%., 1H, NH), 7.91 (5, 2H, CH), 7.77 (5, 2H,CH), 6.45 (++5, 2JPtH = 34 X$, :S%., 1H, NH), 3.40–3.20 (4, 8H, NCH2), 1.70–1.40 (4, 12H, CH2).C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.&1*4"'#1+& F +4#+% 4#,&)*'-)%,.*4#,&) (1:1 "* *9_#4:) )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.NC5H10Cl3.42; N, 12.10. -&J5#)*: C, 30.43; H, 3.45; N, 12.16%.