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PRESENTED BY
DIVYA V
1ST M PHARM
PHARMACEUTICAL CHEMISTRY
PRESENTED BY
DIVYA V
1ST M PHARM
PHARMACEUTICAL CHEMISTRY
 1D NMR
 2D NMR
 COSY
 NOESY
 It is a type of spectroscopy where the energy
states of spin-active nucleus placed in a
static magnetic field are interogated by
inducing transitions between the states via
radiofrequency irradiation.
 Contain sequence of radio frequency pulses.
 Plot-Chemical shift vs radiofrequency.
 Includes regular H-proton spectrum, C-13
spectra.
 PRINCIPLE
 Consist of 2 sections
#Preparation
#Detection
PREPARATION-A 90 ͦ pulse is applied which
rotates the equilibrium magnetization along
Z axis to Y axis
 This induces a signal in receiver coil.
 The signal decays due to T2 relaxation & is
called as FREE INDUCTION DECAY(FID)
 FOURIER TRANSFORMATION to get final 1D
spectrum.
TYPES
 REGULAR
 Sample reaches equilibrium.
 RF signal is transmitted.
 Signal is evolved(FID)
 Fourier transformation
 Final spectra is obtained
 DECOUPLED
 Heteronuclear coupling from another nucleus
with magnetic spin causes the signal to split
& sensitivity to fall.
 Apply decoupling is necessary.
 GATED DECOUPLING
 Apply decoupling during relaxation time.
 OTHER METHODS OF DECOUPLING,
-Off resonance
-Solvent suppression
-Deuterium substitution
 Nuclear overhauser effect
 The local field of one nucleus is
affected by another nucleus.
 Causes reduction in intensity
of signal.
 1D NMR SPECTRAL ANALYSIS
 Contain following information for analysis,
#Chemical shift
#Spin-Spin coupling
#Intensity
INTERPRETATION OF H-NMR
 No:of signals-Indicates how many different
kinds of protons are present.
 Position of signals: Chemical shift.
 Intensity of signals: No:of protons.
 Splitting of signals: No:of nearby nuclei
usually protons.
 ANALYSIS OF C-13 NMR
E.g. Propyl acetate
2D NMR
DEFINITION
 It gives data plotted in space defined by 2
frequency axes rather than one.
 PRINCIPLE
 A 90 ͦ pulse is provided to sample & then
depending upon the type again a 90 ͦ pulse
is provided & this time, signal FID is
measured.
 STAGES OF 2D NMR
TYPES
# HOMONUCLEAR THROUGH-BOND
CORRELATION METHODS
*COSY *ECOSY *TOCSY *INADEQUATE
# HOMONUCLEAR THROUGH BOND-
CORRELATION METHODS
*HSQC *HMBC *HETCOR
# THROUGH SPACE CORRELATION METHODS
*NOESY *ROESY
HOMONUCLEAR
 2 Frequency is provided to same nuclei in
sample.
COSY
 Used to identify spins which are coupled to
each other.
 2 axes are proton chemical shift.
 Consist of 2 types of peaks
* Diagonal peaks
* Cross peaks
 Diagonal peak-Corresponds to normal 1D
spectrum.
 Cross peak-Spin-Spin coupling.
 Cross peaks appears in matched positions in
the diagonal peaks.
TYPES
 A)NORMAL COSY PULSE SEQUENCE
 B)COSY 45 ͦ PULSE SEQUENCE
 C)LONG RANGE COSY PULSE SEQUENCE
 D)MQF COSY PULSE SEQUENCE
 E.G. GERANIOL
2
13
4
5
6
7
CH3
8
CH3
9
CH3
10
OH
 E.G. ASPIRIN
1
2
6
3
5
4
7
O OH
O
8 9
O
CH3
Fig;Cosy spectrum of aspirin
THROUGH SPACE CORRELATION METHODS
NUCLEAR OVER-HAUSER EFFECT
SPECTROSCOPY(NOESY)
 Developed to observe NOE in 2D
spectroscopy.
 Useful in structural elucidation.
Fig : Pulse in NOESY
 E.g. 12,14-ditbutylbenzochrysene.
Fig NOESY spectrum 12,14ditbutylbenzochrysene.
REFERENCES
 Spectrophotometric identification of organic
compounds by Silverstein, Barsler and Morril.
Fifth edition;227-267.
 Instrumental methods of chemical analysis by
Gurdeep.R.Chatwal and Sham.k.Anand.
Himalaya publishing house:4.73-5.63
 1D and 2D NMR experiment methods by
Dr.Shaoxiong.Wu : April 14:2011
NMR spcetroscopy

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GENERAL PHARMACOLOGY - INTRODUCTION DENTAL.ppt
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NMR spcetroscopy

  • 1. PRESENTED BY DIVYA V 1ST M PHARM PHARMACEUTICAL CHEMISTRY PRESENTED BY DIVYA V 1ST M PHARM PHARMACEUTICAL CHEMISTRY
  • 2.  1D NMR  2D NMR  COSY  NOESY
  • 3.  It is a type of spectroscopy where the energy states of spin-active nucleus placed in a static magnetic field are interogated by inducing transitions between the states via radiofrequency irradiation.  Contain sequence of radio frequency pulses.  Plot-Chemical shift vs radiofrequency.  Includes regular H-proton spectrum, C-13 spectra.
  • 4.  PRINCIPLE  Consist of 2 sections #Preparation #Detection PREPARATION-A 90 ͦ pulse is applied which rotates the equilibrium magnetization along Z axis to Y axis
  • 5.  This induces a signal in receiver coil.  The signal decays due to T2 relaxation & is called as FREE INDUCTION DECAY(FID)  FOURIER TRANSFORMATION to get final 1D spectrum.
  • 6. TYPES  REGULAR  Sample reaches equilibrium.  RF signal is transmitted.  Signal is evolved(FID)  Fourier transformation  Final spectra is obtained
  • 7.  DECOUPLED  Heteronuclear coupling from another nucleus with magnetic spin causes the signal to split & sensitivity to fall.  Apply decoupling is necessary.  GATED DECOUPLING  Apply decoupling during relaxation time.
  • 8.  OTHER METHODS OF DECOUPLING, -Off resonance -Solvent suppression -Deuterium substitution  Nuclear overhauser effect  The local field of one nucleus is affected by another nucleus.  Causes reduction in intensity of signal.
  • 9.  1D NMR SPECTRAL ANALYSIS  Contain following information for analysis, #Chemical shift #Spin-Spin coupling #Intensity INTERPRETATION OF H-NMR  No:of signals-Indicates how many different kinds of protons are present.  Position of signals: Chemical shift.  Intensity of signals: No:of protons.  Splitting of signals: No:of nearby nuclei usually protons.
  • 10.  ANALYSIS OF C-13 NMR E.g. Propyl acetate
  • 12. DEFINITION  It gives data plotted in space defined by 2 frequency axes rather than one.
  • 13.  PRINCIPLE  A 90 ͦ pulse is provided to sample & then depending upon the type again a 90 ͦ pulse is provided & this time, signal FID is measured.
  • 14.  STAGES OF 2D NMR
  • 15. TYPES # HOMONUCLEAR THROUGH-BOND CORRELATION METHODS *COSY *ECOSY *TOCSY *INADEQUATE # HOMONUCLEAR THROUGH BOND- CORRELATION METHODS *HSQC *HMBC *HETCOR # THROUGH SPACE CORRELATION METHODS *NOESY *ROESY
  • 16. HOMONUCLEAR  2 Frequency is provided to same nuclei in sample. COSY  Used to identify spins which are coupled to each other.  2 axes are proton chemical shift.  Consist of 2 types of peaks * Diagonal peaks * Cross peaks  Diagonal peak-Corresponds to normal 1D spectrum.  Cross peak-Spin-Spin coupling.
  • 17.  Cross peaks appears in matched positions in the diagonal peaks. TYPES  A)NORMAL COSY PULSE SEQUENCE
  • 18.  B)COSY 45 ͦ PULSE SEQUENCE  C)LONG RANGE COSY PULSE SEQUENCE
  • 19.  D)MQF COSY PULSE SEQUENCE  E.G. GERANIOL 2 13 4 5 6 7 CH3 8 CH3 9 CH3 10 OH
  • 22. THROUGH SPACE CORRELATION METHODS NUCLEAR OVER-HAUSER EFFECT SPECTROSCOPY(NOESY)  Developed to observe NOE in 2D spectroscopy.  Useful in structural elucidation. Fig : Pulse in NOESY
  • 24. Fig NOESY spectrum 12,14ditbutylbenzochrysene.
  • 25. REFERENCES  Spectrophotometric identification of organic compounds by Silverstein, Barsler and Morril. Fifth edition;227-267.  Instrumental methods of chemical analysis by Gurdeep.R.Chatwal and Sham.k.Anand. Himalaya publishing house:4.73-5.63  1D and 2D NMR experiment methods by Dr.Shaoxiong.Wu : April 14:2011