NMR C [Compatibility Mode].pdf
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Transcript of NMR C [Compatibility Mode].pdf
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8/17/2019 NMR C [Compatibility Mode].pdf
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NMR
13C NMR
SPECTROSCOPY
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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
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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
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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#
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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#
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NMR opling 13C te-"adap 1#
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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#
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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-
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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#
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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#
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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
$e-ki-aan δ atom C (ppm)
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NMR
Aldehydes
Ket!es
A"#ds A$#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%
$e-ki-aan δ atom C (ppm)
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NMR
!#tr#les
&"#d &!hydr#des&"#d "hlr#des
&$#des
esters
"&r(yl#" &"#ds
&ldehydes
-*!s&t*r&ted ,et!es
,et!es
220 200 180 160 140 120 100 ++$
$e-ki-aan δ atom C (ppm)
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NMR
200 150 100 50 0
ROON
%CO)%
HO-CH2-CH2-CH3" ( &
Conto" spekt-m
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NMR Conto" spekt-m
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NMR Conto" spekt-m
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NMR Conto" spekt-m
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NMR Conto" spekt-m
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NMR Conto" spekt-m
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NMR
Cl
Cl&
&
(
(
"
"
Conto" spekt-m
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NMR Conto" spekt-m
Cl
Cl
&"
&(d
d
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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 $lse Se?enes
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NMR G$*
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NMR G$*
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NMR IN'$*
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NMR '$*
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NMR '$*