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BY (11) 13262
(13) C1
(46) 2010.06.30
(19)
(12)
(51)
(2009)
C 07D 209/00
C 07D 333/00
C 07D 263/00
C 09K 11/06
(54)
,
,
(21)
(22) 2008.06.04
(43) 2010.02.28
(71)
:
: a 20080730
(73)
"
-
" (BY)
"
(56) WO 01/40401 A1.
. //
i
ii
i.
.- 2005.- 5.- . 5-8.
RU 2296756 C2, 2007.
US 2719155, 1955.
US 4105446, 1978.
SU 406364, 1973.
" (BY)
(72)
:
:
;
;
;
(BY)
.
.
-
(57)
1.
I
BY 13262 C1 2010.06.30
R
1
O
O
X
NR
SO2;
R - , C2H5, C6H13
C6H5;
R1 - ,
,
N(CH
)
6 13
3 2, NHC4H9
,
X
,
N
N
X
NHC6H13;
NR, R1
(I)
,
.
2.
. 1,
II
,
O
O
N
N
N
,
(II)
R
R
3.
, C2H5, C6H13
C6H5.
,
. 1,
III
5,5-
BY 13262 C1 2010.06.30
R1
O
O
,
(III)
NHC6H13.
. 1,
-
S
O
R1
4.
,
N
N
6
13,
O
N(CH3)2, NHC4H9
2R1
O
O
,
H
X
H
X
NR
SO2;
R - , C2H5, C6H13
C6H5;
R1 - ,
6 13, N(CH3)2, NHC4H9
,
X
40-50 °
4-24
.
5.
. 4,
.
6.
. 4,
.
NHC6H13;
NR,
R1
,
,
-
,
-
,
,
,
-2-
I
R
1
O
O
,
N
N
X
(I)
X - NR (II), S(O)2 (III);
R1 - , R - (II ), 2 5 (II ), 6 13 (II ), 6 5 (II );
R1 - (IIIa),
6 13 (III ), N(CH3)2 (III ), NHC4H9 (III ), NHC6H13 (III );
,
X
NR, R1
,
,
,
,
I,
(II
.
)
O
O
N
N
N
,
(II)
R
R
-( )-
(II ),
2
5
(II ),
6
5,5-
13
(II ),
6
5
I,
2
(II ),
(III
)
BY 13262 C1 2010.06.30
R1
O
O
,
N
N
S
O
(III)
O
R1 - H (IIIa), OC6H13 (III ), N(CH3)2 (III ), NHC4H9 (III ), NHC6H13 (III ).
,
,
-
,
.
,
,
,
,
[1-6].
-
,
[2],
.
3,7-
(
2,7-
)
,
,
-
.
N-
N-
(II
)
-
(III )
.
,
1
(III
)
.
(V
2-
(IV)
40-50 °
4-24
2,
VI)
-
) - 546-547,5
-
,
I,
1
.
II (
), III ( , )
447,5-465
II(
), III (
,
III (
.
)
516,5-550,5
.
II (
.1
), III (
)
2.
.
.
)
II (
2,7):
-[2-(
-2-
)-( )-
]-
I,
O
(IV)
O
O
N
H
H
N
R
(V)
3
,
, 40-50
-
BY 13262 C1 2010.06.30
O
O
N
N
N
R
1
5 (II ),
R-
(II ), 2
1
2,7-[2-(
300
(6,70
(4,02
40-50 ° .
, 5,0
8
, 3,0
(II)
6
13
-2(1,34
.)
(II ),
6
5
(II ).
)-( )]-9
)9
-2,7446
(3,35
, 2,5
3,0
.
40-50 ° ,
.)
,
(II ).
5,0
.
, 362
.) 2.
217
5
(
10,0
.
),
,
,
.
.
.
503
(83 %). .
HH
. 319-319,5 ° (
.);
(
-d6, 500
), δ,
.: 7,26 ( , 2 , J 16,5 ,
-), 7,33 ( , 2 , Jop = 7,0
,J
2,3
, 5,6′/6,6′
), 7,35 ( , 2 , j
7,3 , J 2,8 , 5,5′/6,
), 7,57 ( , 2 , J
8,0 , 4,4′/7,7′
),
op
7,62 ( , 2 , J
8,0 , J
1,0 , 4,4′/7,7′
), 7,68 ( , 2 , J
8,0 , 3,6), 7,81 ( , 2 , 1,8), 7,96 ( , 2 , JHH 16,5
,=
-), 8,12 ( , Jop
8,5 , 2 , 4,5), 11,52 ( , 1H, >NH);
(KBr, v, -1): 3427, 3260, 3070, 3027,
2930, 2883, 2860, 1633, 1620, 1597, 1563, 1537, 1530, 1500, 1467, 1450, 1433, 1350, 1327,
1293, 1280, 1267, 1240, 1180, 1167, 1150, 1113, 1003, 967, 940, 930, 887, 853, 830, 807, 793,
760, 737, 727;
(
, λmax,
(ε, /(
⋅ ): 388,0 (115500), 409,5 (
, 94400).
(
, λmax, , λ = 365,0 ) 460,5;(
.
., λmax, , λ = 365,0 )
548,0, 602,0.
2
2,7-[2-(
-2- )-( )](II
).
.
251-307
(1,0
)
9(N)-2,730,0
.
320
(2,5
,
2,5
.) 2338
(3,0
, 3,0
.)
.
4-16
40-50 ° ,
.
,
, .
,
NaCl
. Na2SO4.
1
(SiO2,
:
)
.
.
2,7-[2-(
-2- )-( )]-9(N)(II ).
144
1
HH
(76 %).
. 309,5-312,0 ° ;
(
-d6, 500
), δ,
.: 1,41 ( , 3 , J 7,0 ,
HH
op
7,5
, >NCH2-), 7,40 ( , 2 , J
7,3
, J
1,3
, 5,5′/6,6′3), 4,60 ( , 2 , J
), 7,43 ( , 2 , J
7,5 , J
1,5 , 5,5′/6,6′
), 7,54 ( , 2 ,
J 16,5 , = -), 7,67 ( , 2 , J
8,5 , J
1,0 , 3,6), 7,75 ( , 2 , J
8,5 , J
0,5 , 4,4′/7,7′
), 7,76 ( , 2 , J
8,5 , J
0,5 , 4,4′/7,7′HH
), 8,03 ( , 2 , J 16,0 , = -), 8,19 ( , 2 , 1,8), 8,25 ( , 2 ,
J
8,0
, 4,5);
(KBr, v, -1): 3070, 3063, 3030, 2963, 1640, 1567, 1560,
1533, 1493, 1467, 1450, 1440, 1367, 1347, 1333, 1300, 1283, 1240, 1230, 1190, 1180, 1160,
4
BY 13262 C1 2010.06.30
1147, 1107, 1087, 1060, 1003, 970, 930, 883, 853, 833, 823, 817, 797, 783, 757, 737, 723, 703;
(
, λmax,
(ε, /(
⋅ ))): 389,5 (129100), 413,5 (
, 108800).
, λmax, , λ = 365,0 ) 464,5; (
.
., λmax, , λ = 365,0 ) 516,5, 547,5.
2,7-[2-(
-2- )-( )]-9(N)(II ).
144
1
HH
(52 %). . . 42,6-46,0 ;
(
-d6, 500
), δ,
.: 0,83 ( , 3 , J 7,0 ,
HH
7,1 , >NCH2CH2-), 4,52 ( , 2 , JHH 7,3 ,
3), 1,1-1,3 ( , 6 , 2-), 1,84 ( , 2 , J
>NCH2-), 7,39 ( , 2 , J
7,3
, J
1,3
, 5,5′/6,6′
), 7,42 ( , 2 , J
HH
7,3 , J
1,3 , 5,5′/6,6′
), 7,51 ( , 2 , J 16,0 , = -), 7,65 ( , 2 ,
J
8,0 , J
1,0 , 3,6), 7,73 ( , 2 , J
8,5 , 4,4′/7,7′
),
HH
7,75 ( , 2 , J
8,5 , 4,4′/7,7′
), 8,03 ( , 2 , J 16,0 , = -), 8,19 ( , 2 ,
-1
1,8), 8,25 ( , 2 , J
8,0
, 4,5).
(KBr, v,
): 3427, 3073,
3040, 2973, 2933, 2867, 2757, 2727, 2630, 1660, 1640, 1613, 1597, 1567, 1547, 1540, 1497,
1457, 1390, 1383, 1370, 1333, 1287, 1243, 1203, 1183, 1167, 1113, 1043, 1023, 1003, 963, 947,
933, 857, 843, 827, 793, 767, 737.
(
, λmax,
(ε, /(
⋅ ): 389,0 (84100), 413,0
, 69400).
(
, λmax, , λ X = 365,0 ) 464,0; (
.
., λmax, ,
λ = 365,0 ) 546,0, 600,5.
2,7-[2-(2)-( )]-9(N)(II ).
138
(78 %). . . 306,5-309,5 (
.); 1
(
-d6, 500
), δ,
.: 7,32-7,45 ( ,
, 5,5′,6,6′
), 7,63 ( , 1 , J
6,5 , J
1,3 , 4-Ph), 7,65-7,80 ( , 8 ,
HH
4,4′,7,7′
+ 2,3,5,6- h),7,77( , 2H, J 16,0 , = -), 7,86 ( , 2 , J
8,0 ,
J
1,0 , 3,6), 8,00 ( , 2 , JHH 16,0 , = -), 8,31 ( , 2 , 1,8),
-1
8,37 ( , 2 , J
8,0 , 4,5).
(K r, v,
): 3072, 3039, 2971, 2941, 2872,
1639, 1600, 1571, 1534, 1505, 1456, 1430, 1354, 1321, 1305, 1292, 1250, 1233, 1207, 1184,
1171, 1154, 1118, 1085, 1039, 1017,975,944,905, 885, 869, 846, 833, 807, 770, 754, 708.
, λmax,
(ε, /(
⋅ ): 386,0 (192900), 408,5 (
, 156000).
, λmax,
, (λEX = 365,0
) 457,5; (
.
., λmax,
, λ = 365,0 ) 477,5, 547,5,
604,0.
)
3,7- -[2-(
-2- )-( )]-5,5I,
III ( )
R1
O
(IV)
O
O
N
H
S
H
,
, 40-50
O
O
(VI)
R1
O
O
N
N
S
O
R1 3,730,0
.
O
2 (III)
(IIIa), OC6H13 (III ), N(CH3)2 (III ), NHC4H9 (III ), NHC6H13 (III ).
3
-[2-(
-2- )-( )]-5,5(III )
272
(1,0
) 5,5-3,7.
320
(2,5
, 2,5
.)
338
(3,0
, 3,0
.)
.
40 ° ,
,
,
5
24
BY 13262 C1 2010.06.30
,
.
,
-
.
467
(93 %). . . >350 ° (
.); 1
(
-d6, 500
), δ,
.:
7,42 ( , 2 , JHH 16,5 , = -), 7,41 ( , 4 , 5,5′,6,6′
), 7,71 ( , 2 , J
8,0
, J 1,0
, 4,4′/7,7′
), 7,75 ( , 2 , J
7,0
, J
1,0
, 4,4′/7,7′), 7,95 ( , 2 , J
8,0 , J
1,0 , 2,8), 7,98 ( , 2 , JHH
16,5
, = -), 8,43 ( , 2 , J
= 9,0
, 1,9), 8,44 ( , 2 , 4,6-1
);
(KBr, v,
): 3073, 3043, 2943, 2873, 1647, 1603, 1540, 1460, 1410,
1360, 1343, 1317, 1297, 1253, 1213, 1197, 1177, 1123, 1090, 1073, 1017,980,967, 950, 890,
870, 857, 817, 770, 757, 730.
(
, λmax,
(ε, /(
⋅ ): 372,5 (95400), 395,0 (
,
77500).
(
, λmax, , λ = 365,0 ) 447,5.
4
1-3,7-[2-(
-2- )-( )]-5,5(III ).
372
(1,0
) 1-5,5-3,715,0
.
270
(2,0
,
2,0
.) 290
(2,0
, 2,0
.)
5,0
.
.
40-50 °
16 ,
.
,
,
, 5 %,
l,
pH
.
530 (88 %).
. 269-271 ° ; 1
(
-d6,500
), δ,
.: 0,91 ( , 3 ,
, - 3), 1,31-1,45 ( , 4 , - 2-), 1,54 ( , 2 , JHH 7,3 , - 2-), 1,93 ( , 2 , JHH
5,8 , 5,5′/6,6′
),
2
2-), 7,37 ( , 2 , J
2-), 4,34 ( , 2 , HH
, J 7,0 , 5,5′/6,6′
), 7,55 ( , 1 , J 16,5 , = -), 7,65 ( , 1H,
, = -), 7,72 ( , 2 , J 8,0 , 4,4′,7,7′
), 7,76 ( , 2 , J 7,0 ,
), 7,83 ( , 1H, 2/4/6), 7,85 ( , 1H, JHH 15,5 , = -),
HH
, J = 15,5 , = -), 8,07 ( , 1 , 2/4/6), 8,11 ( , 1H, J 8,0 ,
), 8,23 ( , 1 , J 6,5
, 8/9), 8,51 ( , 1H, 2/4/6).
(KBr, v, -1): 3077, 3043, 2970, 2943, 2883, 2873, 1643, 1597, 1583,
1537, 1453, 1430, 1413, 1353, 1310, 1247, 1193, 1167, 1120, 1043, 1013, 977, 947, 900, 887,
863, 840, 773, 757, 730.
(
, λmax,
(ε, /(
⋅ ): 389,5 (95600), 412,5 (
,
83400).
(
, λmax, , λ = 365,0 ) 465,0.
5
l-(N,N)-3,7- -[2-(
-2- )-(E)]-5,5(III )
1-(N)-3,7-[2-(
-2- )-( )]-5,5(III , ).
.
315-371
(1,0
) 1-( )-5,5-3,715,0
.
270
(2,0
, 2,0
.) 290
(2,0
, 2,0
.)
5,0
. .
40-50 °
16 ,
.
,
,
.
,
NaCl
. Na2SO4.
(SiO2,
:
).
.
.
J 7,0
6,8 , 7,42 ( , 2
JHH 16,5
4,4′,7,7′
7,86 ( , 1
8/9HH
6
BY 13262 C1 2010.06.30
l-(N,No)-3,7- -[2-(
-2- )-(E)]-5,51
(III ).
442
(81 %).
. 335-336 ° ;
(
-d6, 500
),
5,
.: 2,87 ( , 6 , - 3), 7,40 ( , 2 , J
7,8 , 5,5′/6,6′
), 7,43 ( , 2 , J
7,5 , 5,5′/6,6′
), 7,60 ( , 1 , JHH 16,0 , = -), 7,65 ( , 1 , JHH 16,5 ,
-), 7,74 ( , 2 , J
7,5 , 4,4′/7,7′
), 7,78 ( , 2 , J
= 7,5 , 4,4′/7,7′), 7,90 ( , 1 , 2/4/6), 7,92 ( , 2 , JHH 16,0 , = -), 8,17 ( ,
1H, 2/4/6), 8,18 ( , 1 , J
5,5
, 8/9), 8,33 ( , 1 , J
-1
8,0 , 8/9), 8,54 ( , 1H, 2/4/6);
(KBr, v,
): 3077,
3043, 3003, 2967, 2940, 2883, 2853, 2800, 1647, 1597, 1577, 1547, 1537, 1477, 1457, 1410,
1357, 1303, 1250, 1210, 1193, 1170, 1120, 1057, 1017, 983, 950, 900, 870, 843, 773, 757, 737;
(
, λmax,
(ε, /(
⋅ ): 362,0 (68900), 401,0 (
, 60300).
, λmax, , λ = 365,0 ) 549,0.
1-(N)-3,7-[2-(
-2- )-( )]-5,5(III ).
470
(82 %).
.327-329 ° ; 1
(
-d6, 500
), δ,
.:
HH
1,02 ( , 3 , J 6,8 , - 3), 1,54 ( , 2 , - 2-), 1,78 ( , 2 , -NCH2CH2-), 3,44 ( , 2 ,
-NCH2-), 5,85 ( , 1 , -NH-), 7,37-7,47 ( , 5 , 5,5′/6,6′
+ 2/4/6), 7,43 ( , 1 , JHH 17,0 , = -), 7,50 ( , 1 , JHH 17,0 , = -), 7,64 ( , 1 , 7,82 ( ,
, 2/4/6), 7,70 ( , 2 , J 6,5 , 4,4′/7,7′
), 7,75 ( , 2 , J
6,5 , 4,4′/7,7′
), 7,90 ( , 1 , JHH = 17,0 , = -), 7,94 ( , 1 , JHH = 17,5 ,
-), 8,11 ( , 1 , J
7,0
, 8/9), 8,27 ( , 1H, J
8,0
, 8/9-1
), 8,37 ( , 1 , 2/4/6).
(KBr, v,
): 3413, 3077, 3037,
2977, 2940, 2880, 2867, 1637, 1590, 1570, 1543, 1490, 1470, 1450, 1440, 1420, 1350, 1290,
1237, 1213, 1183, 1157, 1150, 1113, 1087, 1063, 1007, 970, 943, 893, 880, 857, 837, 817, 760,
740, 717.
(
, λmax,
(ε, /(
⋅ ): 352,0 (79200), 434,5 (57900).
, λmax, , λ = 365,0 ) 546,0.
1-(N)-3,7-[2-(
-2- )-( )]-5,51
(III ).
487
(81 %). . . 278-280 ° ;
(
-d6, 500
), δ,
.: 0,90 ( , 3 , JHH = 6,8 , - 3), 1,29-1,40 ( , 4 , - 2-), 1,46 ( , 2 , JHH 7,3 , - 2-),
1,71 ( , 2 , JHH 7,4 , - 2-), 3,15-3,55 ( , 2 , -NCH2-), 6,20 ( , 1 , JHH 3 , -NH-), 7,40
,2 ,J
7,5 , 5,5′/6,6′
), 7,44 ( , 2 , J 8,0 , 5,5′/6,6′
),
HH
HH
7,46 ( , 1 , 2/4/6), 7,62 ( , 1 , J 16,5 , = -), 7,64 ( , 1H, J 16,5 ,
-), 7,75 ( , 2 , J
7,8 , J
3,5 , 4,4′/7,7′
), 7,78 ( , 2 , J
7,5
HH
, 4,4′/7,7′
), 7,82 ( , 1H, 2/4/6), 7,93 ( , 1 , J 16,0
,
-), 7,95 ( , 1 , JHH 16,5 , = -), 8,18 ( , 1 , J
8,0 , 8/9), 8,27 ( ,
,J
8,5 , 8/9), 8,55 ( , 1 , 2/4/6);
(KBr, v, -1):
3453, 3083, 3043, 2970, 2943, 2870, 1643, 1600, 1577, 1547, 1537, 1497, 1477, 1453, 1423,
1357, 1303, 1250, 1217, 1190, 1167, 1157, 1117, 1097, 1067, 1013, 977, 947, 900, 867, 830,
770, 753, 727;
(
, λmax,
(ε, /(
⋅ ): 344,5 (31000), 439,5 (20700).
(
, λmax, , λ X = 365,0 ) 547,5.
(II , III ) , (III ) , (III
),
,
,
,
,
,
.
.
5,5',
-2- -( )75 %,
,
,
.
7
BY 13262 C1 2010.06.30
. 1.
II (
. 2.
III(
).
).
I
II
II
II
II
IIIa
III
III
III
III
,λ ,
/(
)
388,0 (115500)
409,5 (94400)
389,5 (129100)
413,5 (108800)
389,0 (84100)
413,0 (69400)
386,0 (192900)
408,5 (156000)
372,5 (95400)
395,0 (77500)
389,5 (95600)
412,5 (83400)
362,0 (68900)
401,0 (60300)
352,0 (79200)
434,5 (57900)
344,5 (31000)
439,5 (20700)
(ε,
.
.),
460,5
(548,0, 602,0)
464,0
(516,5, 547,5)
464,0
(546,0, 600,5)
457,5
(477,5, 547,5, 604,0)
447,5
(525,5, 544,5)
465,0
(548,5, 605,0)
549,0
(538,0, 612,0)
546,0
(546,0, 601,5)
547,5
550,5, 602,0)
8
∆,
72,5
51,0
74,5
50,5
75,0
51,0
71,5
49,0
75,0
52,5
75,5
52,5
187,0
148,0
194,0
111,5
203,0
108,0
BY 13262 C1 2010.06.30
:
1. WO 01/040 401 Al.
2.
. //
i HAH
3. RU 2296756 2, 2007.
4. US 2719155, 1955.
5. US 4105446, 1978.
6. SU 406364, 1973.
i.
.
.
.- 2005.-
.
220034, .
,
.
, 20.
9
5.- . 5-8.
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