Диссертация (1150306), страница 13
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-&J5#)*: C,19.39; H, 4.10; N, 16.73%. Z!>-O!+ FH+*1*/* .&I.#S#)%2OH(MeOH, m/z): 445.095 ([M – Cl]+, FH0%+'#)* 445.082). >C (KBr,NMe[32](Cl).*,5#'()H# "*'*+H, +4d1): 3339(+.-+%'), 3204(+.), 3159(+.-+%')Hb(NdH); 2312(+%') b(C`N); 1674(*0 +%'), 1655(+%') b(C=N);658(+'-c.) f(CdH). AOG 1H (Me2SO-56, f): 8.64 (+, :S%., 1H, NH), 7.86 (+, :S%., 1H, NH2), 7.57(+, :S%., 1H, NH2), 3.07 (+, 6H, NMe2), 2.97 (+, 6H, NMe2), 2.12 (+, 3H, CH3).HNClPtNMe2NPhNNMe2Cl[33](Cl).;H3*567%.B.&I' 104 °C.;H0%+'#)*5'2C13H20N6Cl2OPt•2H2O: C, 27.00; H, 4.18; N, 14.53.
-&J5#)*: C,26.85; H, 4.21; N, 14.34%. Z!>-O!+ FH+*1*/* .&I.#S#)%2OHNH(MeOH, m/z): 436.052 ([M – Cl – NCNMe2]+, FH0%+'#)* 436.045),507.107 ([M – Cl]+, FH0%+'#)* 507.098), 1012.203 ([2M – H –2Cl]+, FH0%+'#)* 1012.189). >C (KBr, *,5#'()H# "*'*+H, +4d1):3416(+%'), 3358(+%'), 3290(+.) b(NdH); 3045(*0 +'), 2995(*0 +'), 2932(+') b(CdH); 2295(+.-+%')b(C`N); 1666(+%'), 1626(*0 +%') b(C=N); 781(+.), 706(+.) f(CdH).
AOG 1H (Me2SO-56, f): 8.88 (+,:S%., 1H, NH2), 8.56 (+, :S%., 1H, NH2), 7.75–7.70 (4, 4H, NH + o-, #-CH), 7.61 (,, 2H, 3-CH),3.13 (+, 6H, NMe2), 2.58 (+, 6H, NMe2).(9<D=7> <P7GED87PEF 8 ()!-[PtCl2(NCNMe2)2] 31. G&+,F*. 1*4"'#1+& 31 (100 414*'()F )%,.*4#,&)# (1 4') 5*9&F'2'% 1 .&+,F*.: &4%5*1+%4& 4 %'% 6 (110 414*'() F )%,.*4#,&)#(10 4' ".% 60 ºC, 4; 2 4' ".% 20 ºC, 6). G&+,F*. *+,&F'2'% )& 6 0 (5'2 4) %'% )& 18 0 (5'2 6) ".%!73!!+**,F#,+,F:TM#J ,#4"#.&,:.#, "*+'# 0#/* .&+,F*.%,#'( :"&.%F&'% ".% "*)%Y#))*4 5&F'#)%%".% 1*4)&,)*J ,#4"#.&,:.#. 8*':0#))H# ,FU.5H# *+,&,1% ".*4HF&'% 3*'*5)H4 (–5 ºC)3'*.*K*.4*4 (1 4'), I&,#4 +4#+(T O#?-/Et2O (1:1 "* *9_U4:) (2 "*.$%% "* 1 4') % +:S%'% F,#0#)%# 12 0 ".% 1*4)&,)*J ,#4"#.&,:.# )& F*I5:3#.HNClPtClNH2NNMe2O34.
;H3*5 63%. B.&I' 162 °C. ;H0%+'#)* 5'2 C5H12N4Cl2OPt: C, 14.64; H,2.95; N, 13.66. -&J5#)*: C, 14.88; H, 3.17; N, 13.48%. Z!>-O!+ FH+*1*/*.&I.#S#)%2 (MeOH:Me2SO = 10:1, m/z): 432.988 ([M + Na]+, FH0%+'#)*432.988),Me453.046([M – Cl + Me2SO]+,FH0%+'#)*453.043),842.989([2M + Na]+, FH0%+'#)* 842.987). >C (KBr, *,5#'()H# "*'*+H, +4d1):3373(*0 +%'), 3281(+.), 3227(+.), 3182(+.) b(NdH); 2966(+'), 2935(+'), 2887(*0 +'), 2818(*0 +')b(CdH);1661(*0 +%'),1636(+%')b(C=N);571(+.),530(+.)f(CdH).B!R(^'T#),:3'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.32.
AOG 1H (Me2SO-56, f): 7.95 (+, :S%., 1H, NH2), 7.89 (+,:S%., 1H, NH2), 7.42 (+, :S%., 1H, NH), 3.00 (+, 6H, NMe2), 2.16 (+, 3H, CH3). 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"#.&,:.#.HNClPtClNPhNMe2ONH235. ;H3*5 94%. B.&I' 158 °C. ;H0%+'#)* 5'2 C10H14N4Cl2OPt: C, 25.43; H,2.99; N, 11.86. -&J5#)*: C, 25.17; H, 2.82; N, 11.74%. Z!>-O!+ FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 490.035 ([M + NH4]+, FH0%+'#)* 490.048), 494.992([M + Na]+, FH0%+'#)* 495.004), 510.963 ([M + K]+, FH0%+'#)* 510.978),962.030 ([2M + NH4]+, FH0%+'#)* 962.063), 967.026 ([2M + Na]+, FH0%+'#)*967.018), 982.996 ([2M + K]+, FH0%+'#)* 982.992), 1439.048 ([3M + Na]+, FH0%+'#)* 1439.032),1455.011 ([3M + K]+, FH0%+'#)* 1455.006), 1911.069 ([4M + Na]+, FH0%+'#)* 1911.047), 1927.036([4M + K]+, FH0%+'#)* 1927.021).
>C (KBr, *,5#'()H# "*'*+H, +4d1): 3442(+%'), 3432(+%')b(NdH); 2961(+'), 2923(+'), 2853(+') b(CdH); 1653(+.), 1636(+.) b(C=N); 782(+'), 705(+'), 668(+')f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 5:1, 2.5/0.5 4') Rf = 0.31. AOG 1H (Me2SO-56, f): 8.36(+, :S%., 1H, NH2), 8.30 (+, :S%., 1H, NH2), 7.62d7.50 (4, 5H, Ph), 7.46 (+, :S%., 1H, NH), 2.71 (+,6H, NMe2). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H %I 4#5'#))* :"&.%F&TM#J+2.#&1$%*))*J +4#+% F )%,.*4#,&)# )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.(9<D=7> <P7GED87PEF 8 %&"'!/()!-[PtCl2(RCN)2] (R = Et, Ph) 26–29. !4#+(&4%5*1+%4& 4 %'% 6 (100 414*'() % 1*4"'#1+& 26–29 (100 414*'() .&+,F*.2'% F )%,.*4#,&)#(3 4').
G&+,F*. *+,&F'2'% )& 3 0 ".% 1*4)&,)*J ,#4"#.&,:.#, "*+'# 0#/* .&+,F*.%,#'(:"&.%F&'% ".% "*)%Y#))*4 5&F'#)%%. gU',H# "*.*S1% ".*4HF&'% 3*'*5)H4 (–5 ºC)3'*.*K*.4*4 (2 "*.$%% "* 1 4') % +:S%'% F ,#0#)%# 12 0 ".% 1*4)&,)*J ,#4"#.&,:.# )&F*I5:3#.!!74!MeClEtNPtHNCl;H3*574%.B.&I' 114 °C.;H0%+'#)*5'2C8H16N4Cl2OPt•!CHCl3: C, 20.64; H, 3.41; N, 11.67.NO36.NHH-&J5#)*: C, 20.81; H, 3.58; N, 11.50%. Z!>-O!+ FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 378.087 ([M d H – 2Cl]+,EtFH0%+'#)* 378.084), 415.068 ([M d Cl]+, FH0%+'#)* 415.061), 468.069 ([M + NH4]+, FH0%+'#)*468.064), 865.082 ([2M d Cl]+, FH0%+'#)* 865.091), 918.093 ([2M + NH4]+, FH0%+'#)* 918.094).>C (KBr, *,5#'()H# "*'*+H, +4d1): 3414(+.), 3350(+%'), 3323(+%'), 3228(+.), 3188(+.) b(NdH);2982(+'-c.), 2948(+'-c.), 2921(+'), 2884(+') b(CdH); 1670(+.), 1637(*0 +%') b(C=N); 588(+'),536(+'-c.) f(CdH).
B!R (^'T#),: 3'*.*K*.4:&$#,*) = 5:1, 2.5:0.5 4') Rf = 0.49. AOG 1H (CDCl3,f): 7.84 (+, :S%., 1H, NH), 4.86 (+, :S%., 2H, NH2), 3.07 (1, 2H, CH2), 2.80 (1, 2H, CH2), 1.95 (+,3H, CH3), 1.40 (,, 3H, CH3), 1.38 (,, 3H, CH3).37.PhClEtNPtHNCl92%.B.&I' 122 °C.;H0%+'#)*5'2C13H18N4Cl2OPt•H2O: C, 29.44; H, 3.80; N, 10.56. -&J5#)*:NO;H3*5NHHC, 29.58; H, 3.51; N, 10.37%. Z!>-O!+ FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 477.081 ([M d Cl]+, FH0%+'#)*Et477.076), 535.039 ([M + Na]+, FH0%+'#)* 535.035), 551.012 ([M + K]+, FH0%+'#)* 551.009),989.129 ([2M d Cl]+, FH0%+'#)* 989.122), 1047.092 ([2M + Na]+, FH0%+'#)* 1047.081), 1063.062([2M + K], FH0%+'#)* 1063.055).
>C (KBr, *,5#'()H# "*'*+H, +4d1): 3427(+.), 3321(+.), 3246(+'),3212(+') b(NdH); 2986(+'), 2944(+'), 2917(+'), 2881(+') b(CdH); 1666(+'), 1626(+%') b(C=N);780(+'), 696(+') f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.55. AOG 1H(CDCl3, f): 7.98 (+, :S%., 1H, NH), 7.64 (5, 2H, o-CH), 7.55 (,, 1H, #-CH), 7.47 (,, 2H, 3-CH), 5.21(+, :S%., 2H, NH2), 3.15 (1, 2H, CH2), 2.80 (1, 2H, CH2), 1.47 (,, 3H, CH3), 1.38 (,, 3H, CH3).C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.&1*4"'#1+& F ^,&)*'# )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.38.MeClPhNPtHNClPh57%.B.&I' 136 °C.;H0%+'#)*5'2C16H16N4Cl2OPt•0.1CHCl3: C, 34.64; H, 2.91; N, 10.04.NO;H3*5NHH-&J5#)*: C, 34.74; H, 2.87; N, 9.90%.
Z!>-O!+ FH+*1*/*.&I.#S#)%2 (MeOH, m/z): 474.092 ([M d 2Cl – H]+,FH0%+'#)*474.084),511.068([M d Cl]+,FH0%+'#)*511.061). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3454(+%'), 3413(+%'), 3264(+.) b(NdH); 3072(+'),2926(+.), 2851(+') b(CdH); 1619(+%') b(C=N); 781(+'), 758(+.), 684(+') f(CdH). B!R (^'T#),:3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.41. AOG 1H (CDCl3, f): 8.60 (5, 2H, Ph), 8.32 (+, :S%.,1H, NH), 7.83d7.50 (4, 8H, Ph), 4.98 (+, :S%., 2H, NH2), 2.03 (+, 3H, CH3).!!75!39.PhClPhNPtHNNOClN;H3*582%.B.&I' 136 °C.;H0%+'#)*5'2C21H18N4Cl2OPt•CHCl3: C, 36.31; H, 2.63; N, 7.70.HH-&J5#)*: C, 36.25; H, 2.53; N, 7.71%.
Z!>-O!+FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 607.032 ([M d H]+,FH0%+'#)* 607.037), 1181.105 ([2M d Cl]+, FH0%+'#)*Ph1181.122), 1215.071 ([2M d H]+, FH0%+'#)* 1215.083), 1239.077 ([2M + Na]+, FH0%+'#)*1239.081). >C (KBr, *,5#'()H# "*'*+H, +4d1): 3489(+%'), 3439(+%'), 3268(+.) b(NdH); 3068(+'),2924(+.), 2853(+') b(CdH); 1654(+%'), 1624(+%') b(C=N); 755(+'), 696(+'), 683(+') f(CdH).
B!R(^'T#),: 3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.63. AOG 1H (CDCl3, f): 8.65 (5, 2H, Ph), 8.45(+, :S%., 1H, NH), 7.77–7.48 (4, 13H, Ph), 5.29 (+, :S%., 2H, NH2).ClClN40. ;H3*5 71%. B.&I' 97 °C. ;H0%+'#)* 5'2 C8H16N4Cl2OPt: C, 21.34;EtPtH, 3.58; N, 12.44. -&J5#)*: C, 21.47; H, 3.52; N, 12.40%. Z!>-O!+NOHEtNFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 378.089 ([M d H – 2Cl]+,HFH0%+'#)* 378.084), 415.066 ([M d Cl]+, FH0%+'#)* 415.061), 451.043NHMe([M + H]+, FH0%+'#)* 451.037), 468.071 ([M + NH4]+, FH0%+'#)*468.064),865.090([2M d Cl]+,FH0%+'#)*865.091),918.089([2M + NH4]+, FH0%+'#)* 918.094), 939.019 ([2M + K]+, FH0%+'#)* 939.023), 1278.129 ([3M d H –2Cl]+, FH0%+'#)* 1278.144), 1351.093 ([3M + H]+, FH0%+'#)* 1351.097).
>C (KBr, *,5#'()H#"*'*+H, +4d1): 3417(+.), 3322(+%'), 3242(+.) b(NdH); 2988(+'), 2948(+'-c.), 2921(+'-c.), 2886(+')b(CdH);1672(+.),1631(*0 +%')b(C=N);608(+'),523(+')f(CdH).B!R(^'T#),:13'*.*K*.4:&$#,*) = 3:1, 1.5/0.5 4') Rf = 0.43. AOG H (CDCl3, f): 7.74 (+, :S%., 1H, NH), 5.06 (+,:S%., 2H, NH2), 3.07 (1, 2H, CH2), 2.80 (1, 2H, CH2), 2.01 (+, 3H, CH3), 1.43 (,, 3H, CH3), 1.38 (,,3H, CH3).ClClPtNEt41. ;H3*5 83%. B.&I' 110 °C. ;H0%+'#)* 5'2 C13H18N4Cl2OPt•H2O: C,Et29.44; H, 3.80; N, 10.56.
-&J5#)*: C, 29.37; H, 3.62; N, 10.66%. Z!>-NHONO!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 513.064 ([M + H]+,HFH0%+'#)* 513.053), 530.091 ([M + NH4]+, FH0%+'#)* 530.080),NPhH535.047([M + Na]+,FH0%+'#)*535.035),551.019([M + K]+,FH0%+'#)* 551.009), 1042.133 ([2M + NH4]+, FH0%+'#)* 1042.125),1047.098 ([2M + Na]+, FH0%+'#)* 1047.081), 1063.063 ([2M + K]+, FH0%+'#)* 1063.055).
>C (KBr,*,5#'()H# "*'*+H, +4d1): 3424(+%'), 3332(+.), 3241(+.) b(NdH); 3064(+'), 2992(+'), 2942(+')b(CdH); 1599(+.) b(C=N); 776(+'), 752(+'), 697(+') f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*) =2:1, 2/1 4') Rf = 0.61. AOG 1H (CDCl3, f): 7.89 (+, :S%., 1H, NH), 7.68 (5, 2H, o-CH), 7.59 (,, 1H,#-CH), 7.51 (,, 2H, 3-CH) (Ph), 5.25 (+, :S%., 2H, NH2), 3.15 (1, 2H, CH2), 2.75 (1, 2H, CH2), 1.47(,, 3H, CH3), 1.38 (,, 3H, CH3).!!76!Cl42. ;H3*5 55%. B.&I' 85 °C. ;H0%+'#)* 5'2 C16H16N4Cl2OPt: C, 35.18;ClNH, 2.95; N, 10.26. -&J5#)*: C, 35.24; H, 2.92; N, 10.13%.
Z!>-O!+PhPtNOHPhFH+*1*/* .&I.#S#)%2 (MeOH, m/z): 546.049 ([M + H]+, FH0%+'#)*546.043), 563.078 ([M + NH4]+, FH0%+'#)* 563.069). >C (KBr,HN*,5#'()H# "*'*+H, +4d1): 3447(+%'), 3351(+%'), 3276(+.) b(NdH);NHMe3193(+.), 3064(+'), 2963(+'-c.), 2924(+'), 2866(+') b(CdH); 1648(+.),1623(*0 +%') b(C=N); 805(+.), 757(+.), 697(+.), 684(+.) f(CdH). B!R (^'T#),: 3'*.*K*.4:&$#,*)= 5:1, 2.5/0.5 4') Rf = 0.39. AOG 1H (CDCl3, f): 8.63 (5, 2H, o-CH), 8.41 (+, :S%., 1H, NH), 7.64–7.49 (4, 4H, Ph), 7.42 (,, 2H, 3-CH), 7.23 (5, 2H, o-CH), 5.10 (+, :S%., 2H, NH2), 2.06 (+, 3H, CH3).43.
;H3*5 70%. B.&I' 128 °C. ;H0%+'#)* 5'2 C21H18N4Cl2OPt: C,ClClNPh41.46; H, 2.98; N, 9.21. -&J5#)*: C, 41.24; H, 2.92; N, 9.39%. Z!>-PhPtO!+ FH+*1*/* .&I.#S#)%2 (MeOH, m/z): 609.108 ([M + H]+,NHONFH0%+'#)* 609.053), 626.136 ([M + NH4]+, FH0%+'#)* 626.080),H631.092NPhH([M + Na]+,FH0%+'#)*631.035),647.066([M + K]+,FH0%+'#)* 647.009), 1234.209 ([2M + NH4]+, FH0%+'#)* 1234.125),1239.174 ([2M + Na]+, FH0%+'#)* 1239.081), 1255.141 ([2M + K]+, FH0%+'#)* 1255.055).
>C (KBr,*,5#'()H# "*'*+H, +4d1): 3417(+%'), 3326(+.), 3206(+.) b(NdH); 3064(+'), 2961(+.), 2934(+')b(CdH); 1625(+%'), 1599(+.) b(C=N); 775(+'), 750(+'), 691(+') f(CdH). B!R (^'T#),:3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.37. AOG 1H (CDCl3, f): 8.70 (5, 2H, o-CH), 8.59 (+,:S%., 1H, NH), 7.72 (5, 2H, o-CH), 7.66–7.49 (4, 7H, Ph), 7.42 (,, 2H, 3-CH), 7.24 (5, 2H, o-CH),5.33 (+, :S%., 2H, NH2). 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"#.&,:.#.5.4.2 !7A;9R Z78-#-7P7AE<=7H<P7GED87PABO DEPQH9D8EF QH<;7AB(II) 44–61(9<D=7> <P7GED87PEF 8 %&"'!/()!-[PtCl2(NCNMe2)2] 30, 31.