NMR C [Compatibility Mode].pdf

8/17/2019 NMR C [Compatibility Mode].pdf

1/27

NMR

13C NMR

SPECTROSCOPY


2/27

NMR

12C tidak aktif(NMR) I = 0

13C memiliki spin, I =1/2

(no massa ganjil)

Signal 13C 000 kalile!i" lema"

di!andingkan1

#

$%&S' *+NMRIS R'%IR'

Range gese-an kimia le!i"

!esa- di!andingkan p-oton0 + 200 ppm

akta $enting *entang 13C NMR

1. elimpa"an di alam da-i 13C keil(1.0 da-i sel-" C)

2. Momen magnet da-i13

C keil


3/27

NMR

engan kat medan magnet sama13C !e-esonansi pada f-ekensi 4ang le!i" -enda" da-i 1#

1H

13C

1.51 * 0 M#6

2.37 * 100 M#6

8.07 * 300 M#6

1.51 * 17.1 M#6

2.37 * 27.0 M#6

8.07 * 87.0 M#6

akta $enting *entang 13C NMR


4/27

NMR

elimpa"an di alam13C keil (1.0

da-i sel-" C)

emngkinanmenemkan da atom

13C !e-se!ela"an padamolekl tnggal keil

opling13C + 13C

N9:

Spekt-a ditentkan ole" kont-i!si !an4akmolekl te-"adap spekt-m masing+masing

"an4a memiliki sat atom 13C

opling13C ; 1#


5/27

NMR

n1 = 5 n1 = 3 n1 = 2 n1 = 1

3 p-oton 2 p-oton 1 p-oton 0 p-oton

a-!onmetil

a-!onmetilen

a-!onmetin

a-!onka-te-ne-

( !e-lak at-an n1 )

(onstanta kopling le!i" !esa- > 100 + 200 #6)

opling 13C te-"adap 1#


6/27

NMR opling 13C te-"adap 1#


7/27

NMR

Metode mm 4ang dignakandalam menentkan spekt-m

13C NMRadala" denganmengi-adiasi sel-" inti

"id-ogen dalam molekl danpada saat 4ang sama

-esonansi C dik-

Mem!t"kan sm!e-f-ekensi -adio seknde-(pendekopling) 4ang diset

te-"adap f-ekensi inti 1#sementa-a sm!e- f-ekensi

p-ime- di set te-"adapf-ekensi inti 13C

f-e?en4.

1H-13C

R so-e 2 R so-e 1

ontinosl4sat-ates"4d-ogens

plse tned toa-!on+13

13C signal (FID) measured

@t"e deople-A

Spekt-a ekopling 1#


8/27

NMR Spekt-a ekopling 1#

$ada metode ini inti"id-ogen @dijen"kanA,

inti 1# !e-otasi sea-a epat anta-ada keadaan spin+n4a (1/2 dan +1/2)dan inti C mengo!se-Basi kopling-ata+-ata te-"adap "id-ogen (dalam"al ini nol)

1# tidak saling kopling dengan 13C

Setiap C mem!e-ikan pnak singlet,spekt-m mda" diinte-p-etasi

(sitasi dimana t-ansisi didae-a" dona-d sama!an4ak dengan pa-d,sema te-jadi sea-a epat)

spekt-m 13C dik-


9/27

NMR

13C kopling

te-"adap1

#

$nakmltiplet dapatsaling oBe-lap

13C dekoplingte-"adap 1#

Spekt-m le!i"mda"diinte-p-etasikan

Spekt-a ekopling 1#


10/27

NMR

q

t t

s s

d d

d

De!e-apa inst-men mempe-li"atkan mltiplisitas da-i pnak padaspekt-a dekopling

s = singlet t = t-ipletd = do!let ? = ?a-tetC9' E

Spekt-a ekopling 1#


11/27

NMR

R-CH3 8 - 30

R2CH2 15 - 55

R3CH 20 - 60

C-I 0 - 40C-Br 25 - 65

C-N 30 - 65

C-Cl 35 - 80

C-O 40 - 80

C C 65 - 90

C=C 100 - 150

C N 110 - 140

110 - 175

R-C-OR

O

R-C-OH

O

155 - 185

R-C-NH2

O155 - 185

R-C-H

O

R-C-R

O

185 - 220

$e-ki-aan δ atom C (ppm)


12/27

NMR

Aldehydes

Ket!es

A"#ds A$#des

%sters A!hydr#des

Ar$&t#" r#!'"&r(!s

)!s&t*r&ted

"&r(! - s+2

Al,y!e

"&r(!s - s+

&t*r&ted "&r(! - s+3

ele"tr!e'&t#.#ty e//e"ts

&t*r&ted "&r(! - s+3

! ele"tr!e'&t#.#ty e//e"ts

C=O

C=O

C=C

C C

200 150 100 50 0

200 150 100 50 0

8 - 30

15 - 55

20 - 60

40 - 80

35 - 80

25 - 65

65 - 90

100 - 150

110 - 175

155 - 185

185 - 220

C-O

C-Cl

C-Br

R3CH R4C

R-CH2-R

R-CH3

RAN%



13/27

NMR

!#tr#les

&"#d &!hydr#des&"#d "hlr#des

&$#des

esters

"&r(yl#" &"#ds

&ldehydes

-*!s&t*r&ted ,et!es

,et!es

220 200 180 160 140 120 100 ++$



14/27

NMR

200 150 100 50 0

ROON

%CO)%

HO-CH2-CH2-CH3" ( &

Conto" spekt-m


15/27

NMR Conto" spekt-m


16/27

NMR Conto" spekt-m


17/27

NMR Conto" spekt-m


18/27

NMR Conto" spekt-m


19/27

NMR Conto" spekt-m


20/27

NMR

Cl

Cl&

&

(

(

"

"

Conto" spekt-m


21/27

NMR Conto" spekt-m

Cl

Cl

&"

&(d

d


22/27

NMR

1. J modulated spin echo experiment (Attached Proton Test

APT)2. INEPT (Insensitive Nuclei Enhanced by Polarization

Transfer)

3. DEPT (Distortionless Enhancement by PolarizationTransfer)

'Fpe-iment sing CompleF $lse Se?enes


23/27

NMR G$*


24/27

NMR G$*


25/27

NMR IN'$*


26/27

NMR '$*


27/27

NMR '$*

Documents

NMR C [Compatibility Mode].pdf