Appendix 4–Spectra Relevant to Chapter 4
324
APPENDIX 4
Spectra Relevant to Chapter 4:
Development of a Tandem Conjugate Addition/Prins Cyclization
JN-4-239b-rxst
March 6
exp1 PROTON
SAMPLE PRESATURATION
date Mar 6 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-4-239~ temp not used
b-rxst-Mar6/PROTON~ gain 28
01.fid spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 25.000 dp y
nt 16 hs nn
ct 16 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.689 DISPLAY
tof 499.7 sp -249.9
tpwr 61 wp 5496.3
pw 4.950 rfl 1001.9
DECOUPLER rfp 0
dn C13 rp -170.6
dof 0 lp -79.4
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 33
dmf 32258 th 13
ai ph
1.00
0.991.00
0.87
1.08
1.00
1.00
1.01
1.000.990.98 1.01
1.02
2.98
1.01
1.02
1.04
1.05
4.03
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
allyl
H
245
Appendix 4—Spectra Relevant to Chapter 4 325
JN-4-239b-rxst
exp1 CARBON
SAMPLE PRESATURATION
date Mar 6 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-4-239~ temp not used
b-rxst-Mar6-carbon~ gain 30
/CARBON01.fid spin 0
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 1700 hs nn
ct 1700 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.660 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.1
pw 4.250 wp 25129.0
DECOUPLER rfl 1902.2
dn H1 rfp 0
dof 0 rp 176.1
dm yyy lp 114.0
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 14806
th 8
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
allyl
H
245
Appendix 4—Spectra Relevant to Chapter 4 326
JN-5-049a-col2
exp1 PROTON
SAMPLE PRESATURATION
date Jan 13 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-049~ temp not used
a-col2/PROTON01.fi~ gain 22
d spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 10.000 dp y
nt 32 hs nn
ct 32 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.698 DISPLAY
tof 499.7 sp -249.9
tpwr 61 wp 5496.6
pw 4.950 rfl 4632.1
DECOUPLER rfp 3627.8
dn C13 rp -78.2
dof 0 lp -82.9
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 42
dmf 32258 th 50
ai ph
5.22
1.001.02
0.97
1.01
1.041.04
1.06
1.06
1.09
3.00
1.09
4.146.20
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Bn
H
Me
247e
Appendix 4—Spectra Relevant to Chapter 4 327
JN-5-049a-col2
exp1 CARBON
SAMPLE PRESATURATION
date Jan 13 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-049~ temp not used
a-col2/CARBON01.fi~ gain 30
d spin 20
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 6400 hs nn
ct 6400 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.662 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.8
pw 4.250 wp 25129.0
DECOUPLER rfl 1901.9
dn H1 rfp 0
dof 0 rp -102.2
dm yyy lp 118.3
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 6000
th 10
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Bn
H
Me
247e
Appendix 4—Spectra Relevant to Chapter 4 328
JN-5-049b-col2
exp1 PROTON
SAMPLE PRESATURATION
date Jan 15 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-04~ temp not used
9b-col2/PROTON01.f~ gain 38
id spin not used
ACQUISITION hst 0.008
sw 6410.3 pw90 7.900
at 2.556 alfa 10.000
np 32768 FLAGS
fb 4000 il n
bs 32 in n
d1 1.000 dp y
nt 8 hs nn
ct 8 PROCESSING
TRANSMITTER fn not used
tn H1 DISPLAY
sfrq 399.797 sp -200.1
tof 399.8 wp 4397.7
tpwr 63 rfl 3707.9
pw 3.950 rfp 2902.5
DECOUPLER rp 28.0
dn C13 lp 0
dof 0 PLOT
dm nnn wc 250
decwave W40_OneNMR sc 0
dpwr 34 vs 91
dmf 29412 th 50
ai ph
4.97
2.01
0.92
1.00
0.98 1.00
1.06
1.093.421.10
2.84
0.95
0.98 1.135.16
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Bn
HMeO
247b
Appendix 4—Spectra Relevant to Chapter 4 329
JN-5-049b-col2
exp1 CARBON
SAMPLE PRESATURATION
date Jan 15 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-04~ temp not used
9b-col2/CARBON01.f~ gain 30
id spin not used
ACQUISITION hst 0.008
sw 25000.0 pw90 6.900
at 1.311 alfa 10.000
np 65536 FLAGS
fb 17000 il n
bs 64 in n
d1 1.000 dp y
nt 8500 hs nn
ct 8500 PROCESSING
TRANSMITTER lb 0.50
tn C13 fn not used
sfrq 100.540 DISPLAY
tof 1530.7 sp -0.7
tpwr 59 wp 20105.0
pw 3.450 rfl 1441.9
DECOUPLER rfp 0
dn H1 rp 122.9
dof 0 lp 0
dm yyy PLOT
decwave w wc 250
dpwr 41 sc 0
dmf 10204 vs 162015
th 10
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Bn
HMeO
247b
Appendix 4—Spectra Relevant to Chapter 4 330
JN-5-053b-col2
exp1 PROTON
SAMPLE PRESATURATION
date Jan 24 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-053~ temp not used
b-col2/PROTON01.fi~ gain 22
d spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 25.000 dp y
nt 4 hs nn
ct 4 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.698 DISPLAY
tof 499.7 sp -249.9
tpwr 61 wp 5496.6
pw 4.950 rfl 4632.1
DECOUPLER rfp 3627.8
dn C13 rp -77.0
dof 0 lp -79.1
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 30
dmf 32258 th 50
ai ph
5.00
1.01
0.98 0.94
1.00
1.001.00
0.99
1.02
1.02
2.97
0.973.93 5.74
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Bn
HMe
247d
Appendix 4—Spectra Relevant to Chapter 4 331
JN-5-053b-col2
exp1 CARBON
SAMPLE PRESATURATION
date Jan 24 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-053~ temp not used
b-col2/CARBON01.fi~ gain 30
d spin 20
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 1650 hs nn
ct 1650 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.662 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.8
pw 4.250 wp 25129.0
DECOUPLER rfl 1901.9
dn H1 rfp 0
dof 0 rp -95.4
dm yyy lp 119.6
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 6000
th 8
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Bn
HMe
247d
Appendix 4—Spectra Relevant to Chapter 4 332
JN-5-055a-col2
exp1 PROTON
SAMPLE PRESATURATION
date Jan 22 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-05~ temp not used
5a-col2/PROTON01.f~ gain 30
id spin not used
ACQUISITION hst 0.008
sw 6410.3 pw90 7.900
at 2.556 alfa 10.000
np 32768 FLAGS
fb 4000 il n
bs 32 in n
d1 1.000 dp y
nt 8 hs nn
ct 8 PROCESSING
TRANSMITTER fn not used
tn H1 DISPLAY
sfrq 399.797 sp -199.9
tof 399.8 wp 4397.7
tpwr 63 rfl 806.4
pw 3.950 rfp 0
DECOUPLER rp 28.4
dn C13 lp 0
dof 0 PLOT
dm nnn wc 250
decwave W40_OneNMR sc 0
dpwr 34 vs 90
dmf 29412 th 50
ai ph
5.031.000.97 1.04
1.03
1.041.07 2.10
1.09 3.04
1.04
1.10
3.11
1.144.20 1.12
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Bn
HMe
247c
Appendix 4—Spectra Relevant to Chapter 4 333
JN-5-055a-col2
exp1 CARBON
SAMPLE PRESATURATION
date Jan 22 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-05~ temp not used
5a-col2/CARBON01.f~ gain 30
id spin not used
ACQUISITION hst 0.008
sw 25000.0 pw90 6.900
at 1.311 alfa 10.000
np 65536 FLAGS
fb 17000 il n
bs 64 in n
d1 1.000 dp y
nt 5000 hs nn
ct 5000 PROCESSING
TRANSMITTER lb 0.50
tn C13 fn not used
sfrq 100.540 DISPLAY
tof 1530.7 sp -0.7
tpwr 59 wp 20105.0
pw 3.450 rfl 1441.9
DECOUPLER rfp 0
dn H1 rp 87.1
dof 0 lp 0
dm yyy PLOT
decwave w wc 250
dpwr 41 sc 0
dmf 10204 vs 30000
th 9
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Bn
HMe
247c
Appendix 4—Spectra Relevant to Chapter 4 334
JN-5-055b-col2
exp1 PROTON
SAMPLE PRESATURATION
date Jan 22 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-05~ temp not used
5b-col2/PROTON01.f~ gain 26
id spin not used
ACQUISITION hst 0.008
sw 6410.3 pw90 7.900
at 2.556 alfa 10.000
np 32768 FLAGS
fb 4000 il n
bs 32 in n
d1 1.000 dp y
nt 8 hs nn
ct 8 PROCESSING
TRANSMITTER fn not used
tn H1 DISPLAY
sfrq 399.797 sp -199.9
tof 399.8 wp 4397.7
tpwr 63 rfl 806.4
pw 3.950 rfp 0
DECOUPLER rp 22.5
dn C13 lp 0
dof 0 PLOT
dm nnn wc 250
decwave W40_OneNMR sc 0
dpwr 34 vs 100
dmf 29412 th 50
ai ph
4.781.00
1.00
1.010.96
0.98
1.960.99
2.87
1.02
3.00
2.011.11 5.42
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Bn
H
Me
247f
Appendix 4—Spectra Relevant to Chapter 4 335
JN-5-055b-col2
exp1 CARBON
SAMPLE PRESATURATION
date Jan 22 2014 satmode n
solvent cdcl3 wet n
file /siena/jni/vn~ SPECIAL
mrsys/data/JN-5-05~ temp not used
5b-col2/CARBON01.f~ gain 30
id spin not used
ACQUISITION hst 0.008
sw 25000.0 pw90 6.900
at 1.311 alfa 10.000
np 65536 FLAGS
fb 17000 il n
bs 64 in n
d1 1.000 dp y
nt 6000 hs nn
ct 6000 PROCESSING
TRANSMITTER lb 0.50
tn C13 fn not used
sfrq 100.540 DISPLAY
tof 1530.7 sp -0.7
tpwr 59 wp 20105.0
pw 3.450 rfl 1441.9
DECOUPLER rfp 0
dn H1 rp 83.1
dof 0 lp 0
dm yyy PLOT
decwave w wc 250
dpwr 41 sc 0
dmf 10204 vs 25000
th 7
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Bn
H
Me
247f
Appendix 4—Spectra Relevant to Chapter 4 336
NH
Cl
MeO
2C
NHTFA
Bn
HBr
247a
Appendix 4—Spectra Relevant to Chapter 4 337
NH
Cl
MeO
2C
NHTFA
Bn
HBr
247a
Appendix 4—Spectra Relevant to Chapter 4 338
JN-5-059a-col2
exp1 PROTON
SAMPLE PRESATURATION
date Mar 6 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-059~ temp not used
a-col2/PROTON01.fi~ gain 24
d spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 25.000 dp y
nt 4 hs nn
ct 4 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.689 DISPLAY
tof 499.7 sp -250.0
tpwr 61 wp 5496.3
pw 4.950 rfl 4635.5
DECOUPLER rfp 3627.7
dn C13 rp -176.3
dof 0 lp -75.4
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 31
dmf 32258 th 50
ai ph
1.00 0.990.941.00
0.991.01
3.06
0.95
3.001.00
0.98
0.98
0.94
1.00
2.87
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Me
HBr
Appendix 4—Spectra Relevant to Chapter 4 339
JN-5-059a-col2
exp1 CARBON
SAMPLE PRESATURATION
date Mar 6 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-059~ temp not used
a-col2/CARBON01.fi~ gain 30
d spin 20
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 1600 hs nn
ct 1600 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.660 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.1
pw 4.250 wp 25129.0
DECOUPLER rfl 1902.2
dn H1 rfp 0
dof 0 rp 173.2
dm yyy lp 105.2
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 16000
th 6
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Me
HBr
Appendix 4—Spectra Relevant to Chapter 4 340
JN-5-061a-col2
exp1 PROTON
SAMPLE PRESATURATION
date Feb 26 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-061~ temp not used
a-col2/PROTON01.fi~ gain 20
d spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 25.000 dp y
nt 4 hs nn
ct 4 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.689 DISPLAY
tof 499.7 sp -250.0
tpwr 61 wp 5496.3
pw 4.950 rfl 4635.5
DECOUPLER rfp 3627.7
dn C13 rp 178.0
dof 0 lp -59.2
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 27
dmf 32258 th 50
ai ph
1.01 0.99
0.92
1.021.00
0.981.00
2.91
1.08
2.990.91
0.891.84 4.06
ppm
12
34
56
78
910
NH
Cl
MeO
2C
NHTFA
Me
H
169
Appendix 4—Spectra Relevant to Chapter 4 341
JN-5-061a-col2
exp1 CARBON
SAMPLE PRESATURATION
date Feb 26 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-061~ temp not used
a-col2/CARBON01.fi~ gain 30
d spin 20
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 1000 hs nn
ct 1000 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.660 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.1
pw 4.250 wp 25129.0
DECOUPLER rfl 1902.2
dn H1 rfp 0
dof 0 rp -175.2
dm yyy lp 113.4
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 6000
th 7
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
NH
Cl
MeO
2C
NHTFA
Me
H
169
Appendix 4—Spectra Relevant to Chapter 4 342
JN-5-061b-col2
exp1 PROTON
SAMPLE PRESATURATION
date Mar 5 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-061~ temp not used
b-col2/PROTON01.fi~ gain 18
d spin 20
ACQUISITION hst 0.008
sw 8000.0 pw90 9.900
at 3.000 alfa 10.000
np 48000 FLAGS
fb not used il n
bs 32 in n
d1 25.000 dp y
nt 4 hs nn
ct 4 PROCESSING
TRANSMITTER lb 0.20
tn H1 fn not used
sfrq 499.689 DISPLAY
tof 499.7 sp -250.0
tpwr 61 wp 5496.3
pw 4.950 rfl 4635.5
DECOUPLER rfp 3627.7
dn C13 rp -166.2
dof 0 lp -100.8
dm nnn PLOT
decwave W40_autox7~ wc 250
991 sc 0
dpwr 41 vs 33
dmf 32258 th 50
ai ph
1.07
1.00
0.89
1.080.96
1.06
0.91 1.02
0.900.90
1.13
2.741.36
0.81
ppm
12
34
56
78
910
HN
4,4'
5,5'
6
7,7'
Cl
2,2'
MeO
2C
NH
TF
AM
e
H1
H3
248
N
H
H
H
HC
l
H
H
H
Me R
no
nO
e
nO
e
1 6 4 e
q
met
hyl
este
r 3 4 a
x 2
2ʼ, 5
eq, 7
eq 5 a
x 7 ax
met
hyl
Appendix 4—Spectra Relevant to Chapter 4 343
JN-5-061b-col2
exp1 CARBON
SAMPLE PRESATURATION
date Mar 5 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-061~ temp not used
b-col2/CARBON01.fi~ gain 30
d spin 20
ACQUISITION hst 0.008
sw 31446.5 pw90 8.500
at 1.042 alfa 10.000
np 65536 FLAGS
fb not used il n
bs 64 in n
d1 1.000 dp y
nt 1000 hs nn
ct 1000 PROCESSING
TRANSMITTER lb 0.50
tn C13 lsfid -4
sfrq 125.660 fn not used
tof 1913.3 DISPLAY
tpwr 63 sp -0.1
pw 4.250 wp 25129.0
DECOUPLER rfl 1902.2
dn H1 rfp 0
dof 0 rp -177.1
dm yyy lp 112.0
decwave w PLOT
dpwr 40 wc 250
dmf 13400 sc 0
vs 6000
th 12
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
N
Cl
MeO
2C
NHTFA
Me
H
H
248
Appendix 4—Spectra Relevant to Chapter 4 344
JN-5-085-col
exp1 PROTON
SAMPLE PRESATURATION
date Apr 14 2014 satmode n
solvent acetone wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-085~ temp not used
-col/PROTON01.fid gain 36
ACQUISITION spin 20
sw 8000.0 hst 0.008
at 3.000 pw90 9.900
np 48000 alfa 10.000
fb not used FLAGS
bs 32 il n
d1 25.000 in n
nt 8 dp y
ct 8 hs nn
TRANSMITTER PROCESSING
tn H1 lb 0.20
sfrq 499.692 fn not used
tof 499.7 DISPLAY
tpwr 61 sp -249.9
pw 4.950 wp 5496.3
DECOUPLER rfl 1001.9
dn C13 rfp 0
dof 0 rp -152.3
dm nnn lp -34.7
decwave W40_autox7~ PLOT
991 wc 250
dpwr 41 sc 0
dmf 32258 vs 4
th 0
ai ph
1.00
3.03
ppm
12
34
56
78
910
O
NF3C
H
OMe
O
Br 265
Appendix 4—Spectra Relevant to Chapter 4 345
JN-5-085-col2
exp1 CARBON
SAMPLE PRESATURATION
date Apr 14 2014 satmode n
solvent acetone wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-085~ temp not used
-col2/CARBON01.fid gain 30
ACQUISITION spin 20
sw 31446.5 hst 0.008
at 1.042 pw90 8.500
np 65536 alfa 10.000
fb not used FLAGS
bs 64 il n
d1 1.000 in n
nt 3000 dp y
ct 3000 hs nn
TRANSMITTER PROCESSING
tn C13 lb 0.50
sfrq 125.661 lsfid -4
tof 1913.2 fn not used
tpwr 63 DISPLAY
pw 4.250 sp -0.1
DECOUPLER wp 27641.4
dn H1 rfl 1902.2
dof 0 rfp 0
dm yyy rp -105.3
decwave w lp 119.8
dpwr 40 PLOT
dmf 13400 wc 250
sc 0
vs 23083
th 1
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
220
O
NF3C
H
OMe
O
Br 265
Appendix 4—Spectra Relevant to Chapter 4 346
JN-5-117
Aug 5, 2014
exp1 PROTON
SAMPLE PRESATURATION
date Aug 5 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-117~ temp 25.0
/PROTON01.fid gain 38
ACQUISITION spin 20
sw 8000.0 hst 0.008
at 3.000 pw90 9.900
np 48000 alfa 10.000
fb not used FLAGS
bs 32 il n
d1 1.000 in n
nt 32 dp y
ct 32 hs nn
TRANSMITTER PROCESSING
tn H1 lb 0.20
sfrq 499.689 fn not used
tof 499.7 DISPLAY
tpwr 61 sp -249.9
pw 4.950 wp 5496.3
DECOUPLER rfl 1001.9
dn C13 rfp 0
dof 0 rp -158.3
dm nnn lp -93.9
decwave W40_autox7~ PLOT
991 wc 234
dpwr 41 sc 8
dmf 32258 vs 7
th 11
ai ph
1.05
1.00
3.56
ppm
12
34
56
78
910
O
NF
3C
H
OM
e
O
D 67-d1
92%
D in
corp
ora
tio
n
Appendix 4—Spectra Relevant to Chapter 4 347
JN-5-117
Aug 5, 2014
exp1 CARBON
SAMPLE PRESATURATION
date Aug 5 2014 satmode n
solvent cdcl3 wet n
file /indy/jni/vnm~ SPECIAL
rsys/data/JN-5-117~ temp 25.0
/CARBON01.fid gain 30
ACQUISITION spin 20
sw 31446.5 hst 0.008
at 1.042 pw90 8.500
np 65536 alfa 10.000
fb not used FLAGS
bs 64 il n
d1 1.000 in n
nt 13000 dp y
ct 13000 hs nn
TRANSMITTER PROCESSING
tn C13 lb 0.50
sfrq 125.660 lsfid -4
tof 1913.3 fn not used
tpwr 63 DISPLAY
pw 4.250 sp -0.1
DECOUPLER wp 25129.0
dn H1 rfl 1902.2
dof 0 rfp 0
dm yyy rp 159.5
decwave w lp 137.8
dpwr 40 PLOT
dmf 13400 wc 234
sc 8
vs 30000
th 5
ai cdc ph
ppm
20
40
60
80
100
120
140
160
180
200
O
NF
3C
H
OM
e
O
D 67-d1
92%
D in
corp
ora
tio
n
Appendix 4—Spectra Relevant to Chapter 4 348