Диссертация (1150306), страница 12
Текст из файла (страница 12)
B!R (^'T#),: 3'*.*K*.4:&$#,*) = 8:1,2/0.25 4'), Rf = 0.60. AOG 1H (Me2SO-56, f): 8.67 (++5, 2JPtH = 34 X$, 1H, NH), 7.8–7.3 (4, 7H, Ph,NH2), 3.13 (1, 7.5 X$, CH2), 1.29 (,, 7.5 X$, CH3) (Et). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'%FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F +4#+% &$#,*)-3'*.*K*.4 )&F*I5:3# ".% 45 ºC.PhH14. ;H3*5 72%. B.&I' 158 °C.
;H0%+'#)* 5'2PhNNHClHClPt NNClOONNHClPhC28H26N6Cl4O2Pt: C, 41.24; H, 3.21; N, 10.31.HH-&J5#)*: C, 41.16; H, 3.42; N, 10.30%. >C (KBr,*,5#'()H# "*'*+H, +4–1): 3494(+.), 3390(+.-+%')b(N&4%5–H); 3210(+., :S%.) b(N%4%)–H•••N); 3070(+'),Ph3058(+'), 3028(*0 +') b(CAr–H); 1654(+.) b(C=N)*1+%4; 1616(*0 +%') b(C=N)%4%); 1598(+%'),1565(+.), 1495(+%') b(C=C)Ar; 1450(+.-+%') b(C=C)Ar % f(C–H)Et; 1428(+) f(N&4%5–H). B!R(^'T#),: 3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.61. AOG 1H (Me2CO-56, f): 9.72 (+, :S%., 1H,NH), 8.03 (5, 2H, o-CH), 7.87 (5, 2H, o-CH), 7.65–7.50 (4, 4H, 3-, #-CH), 7.45 (,, 2H, 3-CH), 7.09(+, :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"#.&,:.#.MeHHMe2NHNNOClNClPtNClClNHHMeO15.;H3*579%.B.&I'176 °C.;H0%+'#)*5'2NC10H24N8Cl4O2Pt•eEt2O•a!-!l3: C, 20.06; H, 4.00; N, 16.63.H-&J5#)*: C, 19.94; H, 4.09; N, 16.73%.
Z!>-O!+ FH+*1*/*.&I.#S#)%2, m/z: 179.014 (NH=C(NMe2)ON=C(NH2)Me + Cl]+,NMe2FH0%+'#)* 179.069), 519.122 ([M – 3Cl]+, FH0%+'#)* 519.130),589.055 ([M – Cl]+, FH0%+'#)* 589.068), 625.030 ([M + H]+,FH0%+'#)*625.045),733.150([M –Cl + NH=C(NMe2)ON=C(NH2)Me]+, FH0%+'#)* 733.169). >C (KBr, *,5#'()H# "*'*+H, +4–1):!69!!3469(*0 +%'), 3395(+.-+%') b(N&4%5–H); 3360(+.-+%') b(N%4%)–H); 2968(+'), 2926(+'), 2893(+'),2872(*0 +') b(CAlk–H); 1655(+%') b(C=N)*1+%4; 1610(*0 +%') b(C=N)%4%); 1469(+%') f(C–H)Et;1426(+.)(C–H)NMe;1406(+%')f(N&4%5–H);623(+'),592(+.)f(C–H).B!R(^'T#),:13'*.*K*.4:&$#,*) = 2:1, 2/1 4') Rf = 0.54.
AOG H (Me2SO-56, f): 6.37 (+, :S%., 2H, NH2), 5.30(+, :S%., 1H, NH), 3.02 (+, 6H, NMe2), 1.76 (+, 3H, CH3). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'%FH.&M#)H ".% 4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F )%,.*4#,&)# )& F*I5:3# ".%1*4)&,)*J ,#4"#.&,:.#.PhCH2HMe2NHNONClNClOPtNClClNHH16.;H3*580%.B.&I'165 °C.;H0%+'#)*5'2NC22H32N8Cl4O2Pt•2H2O: C 32.48, H 4.46, N 13.77. -&J5#)* CH32.64, H 4.31, N 13.87. Z!>-O!+ FH+*1*/* .&I.#S#)%2, m/z:671.190 ([M – 3Cl]+, FH0%+'#)* 671.193), 705.151 ([M – H –NMe22Cl]+, FH0%+'#)* 705.154), 741.127 ([M – Cl]+, 741.131),799.082 ([M + Na]+, 799.089), 1577.172 ([2M + Na]+, 1577.190).H>C (KBr, *,5#'()H# "*'*+H, +4–1): 3452 (*0 +%'), 3398(+%')CH2Phb(N&4%5–H); 3334(*0 +%') b(N%4%)–H); 3062(*0 +'), 3027(+') b(CAr–H); 2969(+'), 2933(+'), 2902(+')b(C–H)Alk; 1653(+%') b(C=N)*1+%4; 1610(*0 +%') b(C=N)%4%); 1494(+.), b(C=C)Ar; 1471(4-+)b(C=C)Ar % f(C–H); 1425(+%') f(N&4%5–H); 753(+.), 708(+%') f(C–H)Ar, 630(+.) f(C–H)Alk.
B!R(^'T#),: 3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.64. AOG 1H (Me2CO-56, f): 7.40 (5, :S%., 2H,o-CH), 7.34–7.21 (4, 3H, 3-, #-CH), 6.15 (+, :S%., 2H, NH2), 5.02 (++5, :S%., 2JPtH 24.5 X$, 1H,NH), 3.46 (+, 2H, CH2), 3.16 (+, 6H, CH3). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".%4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F 4#,&)*'# )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.#.PhHHMe2NHNNOClNClPtNClClNHHPhO17. ;H3*5 85%.
B.&I' 175 °C. ;H0%+'#)* 5'2 C20H28N8Cl4O2Pt: C,N32.06; H, 3.77; N, 14.95. -&J5#)*: C, 32.06; H, 4.07; N, 14.91%.HZ!>-O!+FH+*1*/*.&I.#S#)%2,(NH=C(NMe2)ON=C(NH2)Ph – Ph]+,NMe2207.121m/z:129.012FH0%+'#)*129.077),([NH=C(NMe2)ON=C(NH2)Ph + H]+,FH0%+'#)*+207.124), 643.151([M – 3Cl] , FH0%+'#)* 643.162), 678.120([M – 2Cl]+, FH0%+'#)* 678.131), 713.086 ([M – Cl]+, FH0%+'#)*713.099), 749.063 ([M + H]+, FH0%+'#)* 749.076), 771.040 ([M + Na]+, FH0%+'#)* 771.058),784.017 ([M + K]+, FH0%+'#)* 787.032). >C (KBr, *,5#'()H# "*'*+H, +4–1): 3462 (*0 +%'),3400(+%') b(N&4%5–H); 3329(*0 +%') b(N%4%)–H); 3059(*0 +'), 3030(*0 +') b(CAr–H); 2977(+'),2932(+'), 2879(+') b(C–H)NMe; 1643(+.) b(C=N)*1+%4; 1617(*+%', br) b(C=N)%4%); 1570(+.), 1491(+.),b(C=C)Ar; 1469(4-+) b(C=C)Ar % f(C–H)Me; 1400(+.) f(N&4%5–H); 764(+.), 701(+%') f(C–H)Ar,606(+.) f(C–H)Me.
B!R (^'T#),: 3'*.*K*.4:&$#,*) = 10:1, 2/0.2 4') Rf = 0.54. AOG 1H (Me2CO56, f): 7.9–7.65 (4, :S%., 2H, o-CH), 7.6–7.4 (4, 3H, 3-, #-CH), 6.59 (+, :S%., 2H, NH2), 5.13 (+,!70!!:S%., 1H, NH), 3.24 (+, 6H, CH3). C.%+,&''H, ".%/*5)H# 5'2 G!7, 9H'% FH.&M#)H ".%4#5'#))*4 :"&.%F&)%% .&+,F*.& 1*4"'#1+& F 3'*.*K*.4# %'% &$#,*)# )& F*I5:3# ".%1*4)&,)*J ,#4"#.&,:.#.;#M#+,F& 7, 8 % 11–17 +,&9%'()H )& F*I5:3# ".% 1*4)&,)*J ,#4"#.&,:.# F ,FU.5*4+*+,*2)%% % F .&+,F*.# F 9*'(S%)+,F# *./&)%0#+1%3 .&+,F*.%,#'#J. Z,% F#M#+,F& ,&1Y#+,&9%'()H F .&+,F*.# 1%"2M#/* )%,.*4#,&)& "* 1.&J)#J 4#.# F ,#0#)%# 2 0 (11–17), F ,* F.#421&1 1*4"'#1+H 7 % 8 F 5&))H3 :+'*F%23 .&I'&/&T,+2 I& 2 0. C*4"'#1+ 10 .&I'&/&#,+2 F9*'(S%)+,F# *./&)%0#+1%3 .&+,F*.%,#'#J F ,#0#)%# 3 )#5#'( ".% 1*4)&,)*J ,#4"#.&,:.# %'%I&45 4%)F1%"2M#4)%,.*4#,&)#+*9.&I*F&)%#49*'(S*/*1*'%0#+,F&)#%5#),%K%$%.*F&))H3 ".*5:1,*F.
C*4"'#1+ 9 )# 1.%+,&''%I*F&'+2 % .&I'&/&'+2 F ,#0#)%# 6 0".% 1*4)&,)*J ,#4"#.&,:.#, *) )# 9H' *0%M#) *, ".*5:1,*F /%5.*'%I& % 9H' *3&.&1,#.%I*F&)F +4#+% + )%4%. ; 4&++-+"#1,.# F#M#+,F& 14 )# 9H'* *9)&.:Y#)* 1F&I%-4*'#1:'2.)H3 %K.&/4#),)H3 %*)*F )#+4*,.2 )& ".*F#5#)%# ^1+"#.%4#),& F S%.*1*4 %),#.F&'# )&".2Y#)%2)& FH3*5# 1&"%''2.& % %+"*'(I*F&)%2 .&I'%0)H3 .&+,F*.%,#'#J (MeOH, CH2Cl2, MeCN) % %3+4#+#J.5.3.3 /9DEE:G7A<=7> #-7P7AE<=7H<P7GED87PEF 19–25!4#+( %4%)*1*4"'#1+& (11–17) (60 414*'() % NaCN (17.7 4/, 360 414*'() .&+,F*.2'% FMe2SO-d6 (560 41') ".% 1*4)&,)*J ,#4"#.&,:.# + *9.&I*F&)%#4 %4%)*F 19–25 +**,F#,+,F#))*.?1*)0&)%# ".*$#++& 5#1**.5%)&$%% *,+'#Y%F&'% 4#,*5*4 AOG 1-. 8.*5:1,H 5#,#1,%.*F&'% %*3&.&1,#.%I*F&'% + "*4*M(T +"#1,.*+1*"%% AOG 1- 0#.#I 5 4%) "*+'# ".*F#5#)%2 .#&1$%%,"*+'# 0#/* *3&.&1,#.%I*F&'% %3 4#,*5*4 AOG 13C{1H} (*9M## F.#42 )&1*"'#)%2 ".%4#.)* 2 0).; 4&++-+"#1,.&3 .#&1$%*))H3 +4#+#J )& K*)# %),#)+%F)H3 +%/)&'*F, *,)*+2M%3+2 1 Me2SO-d6,9H'% 5#,#1,%.*F&)H "%1% 1F&I%-4*'#1:'2.)H3 %*)*F +**,F#,+,F:TM%3 &4%5*1+%4*F (5'2 19–25) % 5%4#,%'4*0#F%)H (5'2 23–25).19.
;H3*5 "* AOG 1H 100%. 8#.%*5 "*':.&+"&5& *1*'* 8 +:,. AOG 1HEtONHH(Me2SO-56, f): 7.57 (+, :S%., 1H, NH), 6.31 (+, :S%., 2H, NH2), 2.16 (1, 2H,NNHCH2), 1.76 (+, 3H, CH3), 1.08 (,, 3H, CH3). AOG 13C{1H} (Me2SO-56, f):167.51 (C(Et)(O)(=NH)), 158.23 (C(CH3)(NH2)(=N)), 26.17 (CH2), 20.17 (CH3),Me11.05 (CH3).20. ;H3*5 "* AOG 1H 100%.
8#.%*5 "*':.&+"&5& *1*'* 6 +:,. AOG 1HEtONHNH(Me2SO-56, f): 7.59 (+, :S%., 1H, NH), 7.40–7.15 (4, 5H, Ph), 6.43 (+, :S%.,NHCH2Ph2H, NH2), 3.45 (+, 2H, CH2), 2.17 (1, 2H, CH2), 1.07 (,, 3H, CH3).!71!!AOG 13C{1H} (Me2SO-56, f): 168.75 (C(Et)(O)(=NH)), 157.91 (C(CH2Ph)(NH2)(=N)), 137.89 (*#+oC), 129.54 (3-CH), 129.10 (o-CH), 127.42 (#-CH), 37.67 (CH2Ph), 25.91 (CH2), 11.43 (CH3).21. ;H3*5 "* AOG 1H 100%.
8#.%*5 "*':.&+"&5& *1*'* 5 +:,. AOG 1HEtHONNH(Me2SO-56, f): 7.82 (+, :S%., 1H, NH), 7.75 (5, 2H, o-CH), 7.5–7.4 (4, 3H, 3NHCH % #-CH) (Ph), 6.76 (+, :S%., 2H, NH2), 2.26 (1, 2H, CH2), 1.13 (,, 3H, CH3).AOG 13C{1H}Ph(Me2SO-56,f):168.42(C(Et)(O)(=NH)),156.00(C(Ph)(NH2)(=N)), 132.64 (*#+)-C), 131.24 (#-CH), 129.24 (o-CH), 127.47 (3-CH), 25.91 (CH2),11.52 (CH3).22. ;H3*5 "* AOG 1H 100%. 8#.%*5 "*':.&+"&5& *1*'* 6 +:,. AOG 1HPhHONNH(Me2SO-56, f): 8.41 (+, :S%., 1H, NH), 8.19 (5, 2H, o-CH), 7.84 (5, 2H, o-CH),NH7.55–7.40 (4, 6H, 3-CH % #-CH) (Ph), 7.02 (+, :S%., 2H, NH2). AOG 13C{1H}(Me2SO-56, f): 162.25 (C(Ph)(O)(=NH)), 162.22 (C(Ph)(NH2)(=N)), 156.31 (#-PhCH), 132.68 (#-CH), 131.79 (*#+)-C), 131.35 (*#+)-C), 129.28 (o-CH), 128.99 (o-CH), 128.57 (3CH), 127.69 (3-CH).23.
;H3*5 "* AOG 1H 100%. 8#.%*5 "*':.&+"&5& *1*'* 7 4%). AOG 1HMe2NONH(Me2SO-56, f): 7.02 (+, :S%., 1H, NH), 6.54 (+, :S%., 1H, NH), 5.65 (+,HNNH:S%., 1H, NH), 3.29 (+, 6H, N(CH3)2), 1.82 (+, 3H, CH3). AOG 13C{1H} )#9H' "*':0#) F +%': 9H+,.*/* .&I'*Y#)%2 %4%)& F .&+,F*.#.Me24. ;H3*5 "* AOG 1H 100%. 8#.%*5 "*':.&+"&5& *1*'* 7 4%). AOG 1HMe2NONH(Me2SO-56, f): 7.40–7.17 (4, 5H, Ph), 6.69 (+, :S%., 1H, NH), 6.36 (+, :S%.,HNNHCH2PhOHAOG 13C{1H} )# 9H' "*':0#) F +%': 9H+,.*/* .&I'*Y#)%2 %4%)& F.&+,F*.#.25.
;H3*5 "* AOG 1H 100%. 8#.%*5 "*':.&+"&5& *1*'* 7 4%). AOG 1HMe2NN1H, NH), 5.72 (+, :S%., 1H, NH), 3.45 (+, 2H, CH2), 3.29 (+, 6H, N(CH3)2).N(Me2SO-56, f): 7.74 (5, 2H, o-CH), 7.66–7.35 (4, 3H, 3- % #-CH), 7.18 (+,HNPhH:S%., 2H, NH2), 5.86 (+, :S%., 1H, NH), 3.36 (+, 6H, N(CH3)2).AOG 13C{1H} )# 9H' "*':0#) F +%': 9H+,.*/* .&I'*Y#)%2 %4%)& F.&+,F*.#.!!72!5.4 aD8Q9:7P9A;<HIA<> @<8;I D SH<F9 35.4.1 !7A;9R PEAE-#-7P7AE<=7H<P7GED87PABO DEPQH9D8EFQH<;7AB(II) 32–43(9<D=7> <P7GED87PEF 8 %&"'!-[PtCl2(NCNMe2)2] 30.
G&+,F*. &4%5*1+%4& 4 %'% 6(100 414*'() F )%,.*4#,&)# (3 4', 4) %'% F 3'*.*K*.4# (1 4', 6) "* 1&"'24 F ,#0#)%# 5 4%)5*9&F'2'% 1 "#.#4#S%F*4: .&+,F*.: 1*4"'#1+& 30 (100 41') F )%,.*4#,&)# (1 4', 4) %'% F3'*.*K*.4# (1,5 4', 6). E#.#I 20 4%) .&+,F*.%,#'( :"&.%F&'% ".% "*)%Y#))*4 5&F'#)%% 5**9_U4& 0.5 4'. ?9.&I*F&'+2 "*.*S*1 (%I 4) %'% 4&+'2)%+,HJ *+,&,*1 (%I 6), 1*,*.HJI&1.%+,&''%I*F&'% "*5 F*I5#J+,F%#4 PD. !F#,'*-YU',H# "*.*S1% *,K%'(,.*F&'%, ".*4H'%Et2O (2 "*.$%% "* 1 4') % +:S%'% F ,#0#)%# 12 0 ".% 1*4)&,)*J ,#4"#.&,:.# )& F*I5:3#.HNClPtNMe2NNNMe2Cl;H3*593%.B.&I'152 °C.;H0%+'#)*5'2C8H18N6Cl2OPt•H2O: C, 19.28; H, 4.05; N, 16.87.
![](https://s.studizba.com/z.php?f=/templates/si/i/noavatar.png&w=100&h=100&t=1"){kind=avatar}
