Диссертация (1150306), страница 17
Текст из файла (страница 17)
Z!>-O!+HNPtOCN82. ;H3*5 85%. ;H0%+'#)* 5'2 C18H26N6O2Cl2Pt•1aCHCl3: C, 30.40; H,NHFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 552.169 ([M d NCO – Cl – H]+,NFH0%+'#)* 552.163), 589.145 ([M d NCO]+, FH0%+'#)* 589.140),C5H10N595.172([M d Cl]+,FH0%+'#)*595.169),654.133([M + Na]+,FH0%+'#)* 654.128), 670.107 ([M + K]+, FH0%+'#)* 670.102), 1284.259NO2!90!!([2M + Na]+, FH0%+'#)* 1284.266), 1301.231 ([2M + K]+, FH0%+'#)* 1301.240). Z!>-O!–FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 630.147 ([M d H]–, FH0%+'#)* 630.130), 1260.280 ([2M d H]–,FH0%+'#)* 1260.269). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3437(+.-+%'), 3390(+.-+%') b(NdH);2941(+%'), 2855(+.-+%') b(CdH); 2270(*0 +%') b(OCN); 1651(*0 +%'), 1633(+.-+%') b(C=N);1516(+.-+%') b(N=O)a+, 1345(+%') b(N=O)c. B!R (^'T#),: 3'*.*K*.4:&$#,*) = 3:1, 1.5/0.5 4') Rf= 0.53. AOG 1H (Me2CO-56, f): 9.68 (+, :S%., 1H, NH), 8.35 (5, 2H, CH), 7.85 (5, 2H, CH), 6.43 (+,:S%., 1H, NH), 3.40–3.20 (4, 8H, NCH2), 1.70–1.40 (4, 12H, CH2).5.5.3 +7G:EH7R DEE:G7A7:EF<AAESE =7<A<;< F DEPQH9D8<O 75–82 8 QEH?@9A79P<PPEA7CABO DEPQH9D8EF [83–90](+-MeC6H4SO3)G&+,F*.
8B!C (100 414*'() F &$#,*)# (1 4') 5*9&F'2'% 1 .&+,F*.: $%&)&,)*/*1*4"'#1+& (75–82) (100 414*'() F +4#+% 4#,&)*' – )%,.*4#,&) (1:1 "* *9_#4:, 2 4') % .&+,F*.*+,&F'2'% )& 10 4%) ".% 1*4)&,)*J ,#4"#.&,:.#. 8*+'# ^,*/* %I .#&1$%*))*J +4#+% *,9%.&'%5-41' &'%1F*,: /*4*/#))*/* .&+,F*.&, 1*,*.:T .&I9&F'2'% 1 4' O#?-. C*4"'#1+H [83–90](#MeC6H4SO3) 9H'% 5#,#1,%.*F&)H 4&++-+"#1,.*4#,.%0#+1% F "*':0#))H3 .&+,F*.&3, .#I:'(,&,H".%F#5#)H F ;<ZH7=9 2.NR2ClHNPtH3NO3 SNHNR2NMeR'Y 8E9G7A9A7>R2R'[83](#-MeC6H4SO3)[84](#-MeC6H4SO3)[85](#-MeC6H4SO3)[86](#-MeC6H4SO3)[87](#-MeC6H4SO3)[88](#-MeC6H4SO3)[89](#-MeC6H4SO3)[90](#-MeC6H4SO3)Me2Me2Me2Me2C5H10C5H10C5H10C5H10MeHCNNO2MeHCNNO2[M – +-MeC6H4SO3]+#<CG9AE(<8@7;<AE495.135495.134481.125481.119506.120506.114526.109526.104575.192575.197561.189561.181586.181586.177606.174606.166%<ZH7=< 2.
R&.&1,#.)H# "%1% 1*4"'#1+*F 83–90 F +"#1,.&3 Z!>+-O!-;G.!!91!5.5.4 &EH?@9A79 G7OHE:7GABO <P7G:<REAEFBO DEPQH9D8EF 91–9839;EG7D< 1. &EH?@9A79 DEPQH9D8EF 91–98 7R G7<HD7H=7<A<P7GABO DEPQH9D8EF 30,63 7 <P7GED87PEF 6, 65–67. 8*.*S*1 &.*4&,%0#+1*/* &4%5*1+%4& (6, 65–67) (100 414*'()5*9&F'2'% 1 %),#)+%F)* "#.#4#S%F&TM#4:+2 .&+,F*.: 1*4"'#1+& (30, 63) (100 414*'() F3'*.*K*.4# (2 4') ".% 1*4)&,)*J ,#4"#.&,:.#. E#.#I 7 4%) 1 .#&1$%*))*J +4#+% 5*9&F'2'%.&+,F*.
B67 (100 414*'() F 3'*.*K*.4# (1 4'), "*+'# 0#/* +4#+( *+,&F'2'% )& 1 0 ".% 40 ºC.D&,#4 .&+,F*. 8B!C (100 414*'() F +4#+% 4#,&)*'-)%,.*4#,&) (1:1 "* *9_U4:, 1 4') 5*9&F'2'%1 .#&1$%*))*J +4#+%, 1*,*.:T, "*+'# ^,*/*, *+,&F%'% )& 2 0 ".% 40 ºC. G&+,F*.%,#'( :"&.%'%".% "*)%Y#))*4 5&F'#)%% ".% 1*4)&,)*J ,#4"#.&,:.#. 8*':0#))H# ,FU.5H# *+,&,1%.&+,F*.2'% F +4#+% 3'*.*K*.4 – )%,.*4#,&) (5:1 "* *9_U4:, 2–5 4' F I&F%+%4*+,% *,"*':0*/* 1*4"'#1+&) % .&+,F*.
)&)*+%'% )& +%'%1&/#'(, )&3*52M%J+2 F )#9*'(S*J (5'%)&7 +4, 5%&4#,. 0.7 +4) 1*'*)1#. !4#+( 3.*4&,*/.&K%.*F&'% (^'T#),: 3'*.*K*.4 – )%,.*4#,&) =5:1 "* *9_U4:, 12 4', I&,#4 3'*.*K*.4 – )%,.*4#,&) = 3:2 "* *9_U4:). !*9%.&'% "#.F:TK.&1$%T % .&+,F*.%,#'( :"&.%F&'% ".% "*)%Y#))*4 5&F'#)%% ".% 1*4)&,)*J ,#4"#.&,:.#.8*':0#))H# 1*4"'#1+H 91–98 +:S%'% F ,#0#)%# 1 0 ".% 10 49&..39;EG7D< 2. &EH?@9A79 DEPQH9D8EF 91–98 Q?;^P R<P9V9A7> <PP7<D< A< OHE:7G FDEPQH9D8<O [83–90]+. G&+,F*.
,#,.&9:,%'&44*)%J 3'*.%5& (150 414*'() F 3'*.*K*.4#(0.5 4') 5*9&F'2'% 1 .&+,F*.: +F#Y#".%/*,*F'#))*/* &44*)%J)*/* 1*4"'#1+& (83–90) F3'*.*K*.4# (3 4') % .#&1$%*)):T +4#+( *+,&F'2'% )& 2 0 ".% 40 ºC. G&+,F*.%,#'( :"&.%F&'%".% "*)%Y#))*4 5&F'#)%% ".% 1*4)&,)*J ,#4"#.&,:.#. 8*':0#))H# ,FU.5H# *+,&,1%.&+,F*.2'% F +4#+% 3'*.*K*.4 – )%,.*4#,&) (5:1 "* *9_U4:, 2–5 4' F I&F%+%4*+,% *,"*':0*/* 1*4"'#1+&) % .&+,F*. 9H' )&)#+U) )& +%'%1&/#'(, )&3*52M%J+2 F )#9*'(S*J(5'%)& 7 +4, 5%&4#,.
0.7 +4) 1*'*)1#. !4#+( 9H'& 3.*4&,*/.&K%.*F&)& (^'T#),: 3'*.*K*.4 –)%,.*4#,&) = 5:1 "* *9_U4:, 12 4', I&,#4 3'*.*K*.4 – )%,.*4#,&) = 3:2 "* *9_U4:). !*9%.&'%"#.F:T K.&1$%T % .&+,F*.%,#'( :"&.%F&'% ".% "*)%Y#))*4 5&F'#)%% ".% 1*4)&,)*J,#4"#.&,:.#. 8*':0#))H# 1*4"'#1+H 91–98 +:S%'% F ,#0#)%# 1 0 ".% 10 49&.. ;H3*5H *1*'*65% (*,)*+%,#'()* %+3*5)*/* 1*'%0#+,F& +**,F#,+,F:TM#/* $%&)&,)*/* 1*4"'#1+& 75–82).=&'## :1&I&)H FH3*5H "* 39;EG7D9 1, ,&1 1&1 *,)*+%,#'()* %+3*5)H3 1*4"'#1+*F 30 %63 *)% 9*'(S# )& ~5%, 0#4 "* 39;EG7D9 2.!!92!91.
;H3*5 51%. ;H0%+'#)* 5'2 C13H21N5Cl2Pt•H2O: C, 29.38; H, 4.36; N,NMe2Cl13.18. -&J5#)*: C, 29.47; H, 4.18; N, 13.01%. Z!>-O!+ FH+*1*/*HNPtCl.&I.#S#)%2 (MeOH, m/z): 478.110 ([M d Cl]+, FH0%+'#)* 478.108),NHN536.069 ([M + Na]+, FH0%+'#)* 536.067), 552.042 ([M + K]+, FH0%+'#)*Me2N552.040), 991.182 ([2M d Cl]+, FH0%+'#)* 991.185), 1027.158 ([2M + H]+,FH0%+'#)* 1027.162), 1049.138 ([2M + Na]+, FH0%+'#)* 1049.144),Me1065.112([2M + K]+,FH0%+'#)*1065.118).Z!>-O!–FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 469.025 ([M d NMe2]–, FH0%+'#)* 469.027), 512.061 ([M d H]–,FH0%+'#)* 512.069), 1025.137 ([2M d H]–, FH0%+'#)* 1025.146).
>C (KBr, *,5#'()H# "*'*+H,+4d1): 3300(+.), 3246(+'-c.) b(NdH); 1659(*0 +%'), 1614(+.-+%') b(C=N); 1506(+.-+%') f(NdH).B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.49. AOG 1H (Me2CO-56, f): 8.79 (+, :S%.,1H, NH), 7.40 (5, 2H, CH), 7.27 (5, 2H, CH), 6.06 (+, :S%., 1H, NH), 3.05 (+, 6H, N(CH3)2), 2.72 (+,6H, N(CH3)2), 2.38 (+, 3H, ArCH3).92. ;H3*5 59%.
;H0%+'#)* 5'2 C12H19N5Cl2Pt: C, 28.87; H, 3.84; N, 14.03.NMe2Cl-&J5#)*: C, 29.03; H, 3.76; N, 14.17%. Z!>-O!+ FH+*1*/* .&I.#S#)%2HNPtCl(MeOH, m/z): 464.101 ([M d Cl]+, FH0%+'#)* 464.092), 522.060 ([M + Na]+,NHNFH0%+'#)* 522.051), 538.034 ([M + K]+, FH0%+'#)* 538.025), 963.161Me2N([2M d Cl]+,FH0%+'#)*963.154),1021.119([2M + Na]+,FH0%+'#)*1021.113), 1037.092 ([2M + K]+, FH0%+'#)* 1037.087). Z!>-O!– FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 455.004 ([M d NMe2]–, FH0%+'#)* 455.011), 498.046 ([M d H]–,FH0%+'#)* 498.053), 954.063 ([2M d NMe2]–, FH0%+'#)* 954.073), 997.105 ([2M d H]–, FH0%+'#)*997.115). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3308(+.), 3227(+.) b(NdH); 1664(*0 +%'), 1616(+.+%') b(C=N); 1516(+.-+%') f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.38.AOG 1H (Me2CO-56, f): 8.90 (+, :S%., 1H, NH), 7.53–7.45 (4, 5H, Ph), 6.08 (+, :S%., 1H, NH), 3.04(+, 6H, N(CH3)2), 2.72 (+, 6H, N(CH3)2).
C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".%4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F )%,.*4#,&)# )& F*I5:3# ".% 1*4)&,)*J,#4"#.&,:.#.NMe2Cl93. ;H3*5 60%. ;H0%+'#)* 5'2 C13H18N6Cl2Pt•eH2O: C, 29.53; H, 3.53; N,HNPtCl15.89. -&J5#)*: C, 29.36; H, 3.66; N, 16.05%. Z!>-O!+ FH+*1*/*NH.&I.#S#)%2 (MeOH, m/z): 547.046 ([M + Na]+, FH0%+'#)* 547.046),N563.026 ([M + K]+, FH0%+'#)* 563.020).
Z!>-O!– FH+*1*/* .&I.#S#)%2Me2N(MeOH, m/z): 509.034 ([M d Me]–, FH0%+'#)* 509.033), 523.050 ([M d H]–,FH0%+'#)* 523.049). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3371(+.),CN3217(+.) b(NdH); 2243(+.) b(C`N); 1666(*0 +%'), 1624(+.-+%') b(C=N);!93!!1528(+.-+%') f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.33. AOG 1H (Me2CO56, f): 9.13 (+, :S%., 1H, NH), 7.91 (5, 2H, CH), 7.79 (5, 2H, CH), 6.13 (+, :S%., 1H, NH), 3.02 (+,6H, N(CH3)2), 2.70 (+, 6H, N(CH3)2).94. ;H3*5 55%.
;H0%+'#)* 5'2 C12H18N6O2Cl2Pt•H2O: C, 25.63; H, 3.58;NMe2ClHNN, 14.95. -&J5#)*: C, 25.51; H, 3.53; N, 14.79%. Z!>-O!+ FH+*1*/*PtClNH.&I.#S#)%2 (MeOH, m/z): 509.079 ([M d Cl]+, FH0%+'#)* 509.077),N567.037 ([M + Na]+, FH0%+'#)* 567.036), 583.008 ([M + K]+, FH0%+'#)*Me2N583.010), 1111.079 ([2M + Na]+, FH0%+'#)* 1111.083). Z!>-O!–FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 543.031 ([M d H]–, FH0%+'#)*NO2543.038),1088.086([2M d H]–,FH0%+'#)*1088.093).>C(KBr,*,5#'()H# "*'*+H, +4d1): 3381(+.), 3358(+.-+%') b(NdH); 1659(*0 +%'), 1637(+.-+%') b(C=N);1518(+%') b(N=O)a+, 1348(+%') b(N=O)c. B!R (^'T#),: 3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.37.AOG 1H (Me2CO-56, f): 9.06 (+, :S%., 1H, NH), 8.32 (5, 2H, CH), 7.84 (5, 2H, CH), 6.08 (+, :S%.,1H, NH), 3.01 (+, 6H, N(CH3)2), 2.70 (+, 6H, N(CH3)2).NC5H10Cl11.45.
-&J5#)*: C, 37.49; H, 5.20; N, 11.45%. Z!>-O!+ FH+*1*/*HNPtCl95. ;H3*5 54%. ;H0%+'#)* 5'2 C19H29N5Cl2Pt•H2O: C, 37.32; H, 5.11; N,.&I.#S#)%2 (MeOH, m/z): 558.178 ([M d Cl]+, FH0%+'#)* 558.171),NHN616.132C5H10N([M + Na]+,FH0%+'#)*616.129),1209.278([2M + Na]+,FH0%+'#)* 1209.269). Z!>-O!– FH+*1*/* .&I.#S#)%2 (MeOH, m/z):592.134 ([M d H]–, FH0%+'#)* 592.132), 1185.279 ([2M d H]–, FH0%+'#)*Me1185.271). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3364(+.), 3269(+'-c.)b(NdH); 2932(+%'), 2854(+.-+%') b(CdH); 1649(*0 +%'), 1616(+.-+%') b(C=N); 1516(+.-+%')f(NdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 5:1, 2.5/0.5 4') Rf = 0.53.
AOG 1H (Me2CO-56, f): 9.21(+, :S%., 1H, NH), 7.33 (5, 2H, CH), 7.26 (5, 2H, CH), 6.41 (+, :S%., 1H, NH), 3.45–3.20 (4, 8H,NCH2), 2.39 (+, 3H, CH3), 1.65–1.50 (4, 6H, CH2), 1.20–1.00 (4, 6H, CH2). 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"#.&,:.#.NC5H10ClHNPtClC5H10NNHN96. ;H3*5 49%. ;H0%+'#)* 5'2 C18H27N5Cl2Pt•H2O: C, 36.19; H, 4.89; N,11.72. -&J5#)*: C, 36.40; H, 4.99; N, 11.66%.