Introduction of reacting partners
Recommended procedure
O Assignment of free receptor: /3-cyklodextrine (ID H, DQF-COSY) O Assignment of free ligand: doxepine (ID 1H, DQF-COSY, NOESY)
• Identification of proton resonances of ring A and B
• Determination of major and minor conformation of doxepin
O ID NMR titration: rearrangement of /3-cyclodextrin resonaces upon
interaction =>* identification of inner protons O ID NMR titration: rearrangement of doxepin resonaces upon complexation
=>* estimation of binding mode Q ROESY spectrum of complex: ROE intermolecular contacts O Fitting the titration isotherm
ID XH of ^yclodextrin in D 20
					ľ4h   oh 1						
					i (6 \ 5/   h2\ .j1 hq\j\x yH 3h      0h7° "	7			cd		
	1						e				
	J	f						1 y	b	U	a
			V.						U		Í
	e c c c T	3 3 3 3					c f u c c	3 * J * 3 * i> e	f 1 f c t c 3 C	n 0 n V	1.0196 J
5.0 4.5 4.0 3.5 [ppm]
imb— May 3, 2017       4 / 17
DQF-COSY of ^yclodextrin in D 20
E
Q_ Q.
f
5.0
e c,d b,a
4.0 3.5
4.5 4.0 2-^ (ppm)
Jan Novotný
May 3, 2017       5 / 17
□
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D	
-	
Ill
o
x
-o
INJ
O
[rel]
.....
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p 9
NOESY 700ms of doxepin in D20
NOESY 700ms of doxepin in D20
7.5    /   A \
M   L K J
Jan Novotný
May 3, 2017        10 / 17
ID ľH NMR titration: ^fcyclodextrin
H NMR titration: doxepin
ID *H NMR titration: doxepin
1.9605 1.6154
1.1021
doxepin :(3CD 5:1
3,75:1
1,75:1 1:1
0,75:1
0,2:1 0:1
1.0035
K,L J   | '
1394
0.7815
H-A2
7.4
7.2
7.0
6.8
A
6.6
[ppm]
Find the most perturbed resonances and estimate the time regime of interaction
Jan Novotný
May 3, 2017        14 / 17
ROESY 300ms - doxepin:/iyclodextrin=5:l