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