AMX DAS-M-0608 Manual do Utilizador Página 133

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124
Daten
von
2-(4'-Dimethylaminobenzoyl)-5-dimethylaminobenzoesäure
(64):
O
COOH
(Me)^
^^
^^
N(Me)2
Ausbeute:
25
mg
=
0,07
mmol
=
38%
Smp.:
>220°C
iH-NMR
(DMSO-d6,
200
MHz):
3,00
(s,
lffl,
2
-N(CH3)2);
6,70
(AA'
(J0
=
9,1),
ffl,
H-COO,
H-C(5'));
6,87
(dxd
0o
=
8,6;
Jm
=
2,7),
IH,
H-C(4));
7,05
(d
0m
=
2,6),
IH,
H-C(6));
7,20
(d
(J0
=
83),
IH,
H-C(3));
7,50
(XX1
(Jc
=
9,0),
ffl,
H-C(2'),
H-C(6'));
12,05-13,05
(s
(br.),
COOH).
13C-NMR
(CDC13,
50
MHz):
393
(2
-N(CH3)2);
110,5
(C(3'),
C(5'));
111,7
(C(4)
oder
C(6));
113,1
(C(4)
oder
C(6));
125,2
(Car);
127,9
(Car);
129,6
(Car);
131,1
(C(2'),
C(6'));
133,3
(C(5),
C(4'));
150,4
(Car-N(CH3)2);
152,8
(Car-
N(CH3)2);
168,6
(COOH);
1933
(CO).
IR
(KBr):
2900m
(br.),
2810m
(br.),
2650m,
2540m,
1710m,
1675s, 1635s,
1590s,
1545s,
1525s,
1480s, 1435s,
1415s,
1365s, 1320s,
1290s, 1235s, 1205s,
1175s,
1155s,
1125m,
1075m,
1065m, lOOOw,
945,
930s,
865w,
830m,
815m, 790m,
770m,
740w, 690w,
665w,
650w, 590w,
575w,
510w.
MS
(I>10%):
313(24),
312(M+,
88),
295(12), 268(22), 267(42), 252(12), 251(34), 225(16),
224(62),
208(10),
192(20), 149(17),
148(100),
142(20), 132(10), 120(11),
119(16),
118(10),
105(16),
104(14),
91(11),
79(11), 78(11),
77(18),
42(19).
Daten
von
2-D-4,4'-Bis(dimethylamino)benzophenon
(72):
O
D
NN(Me)2
Ausbeute:
7
mg
=
0,02
mmol
=
12%
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