J. Org. Chem., 1996, 61(25), 8746-8749, DOI:10.1021/jo961600c
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Copyright © 1996 American Chemical Society
SUPPORTING INFORMATION
A Concise Total Synthesis of Dactylol via Ring Closing Metathesis
Alois Fiirstner*and Klaus Langemann
Max-Planck-Institut fir Kohlenforschung
Kaiser-Wilhelm-Platz 1, D-45470 Ml1heim/Ruhr, Germany
Instrumentation and Spectra Formats. NMR: Spectra were recorded on a Bruker AC 200,
AMX 300, AMX 400 or DMX 600 spectrometer in CDCl 3 unless stated otherwise. Chemical
shifts (8) are given in ppm relative to TMS, coupling constants (J) in Hz. The multiplicity in
the
13 C
NMR spectra refers to the geminal protons (DEPT). IR: Nicolet FT-7199,
wavenumbers in cm- 1. MS: Varian CH-5 (70 eV); HR-MS: Finnigan MAT SSQ 7000 (70eV).
UV: Varian Cary 2300, wavelength in nm. Melting points were recorded on a Gallenkamp
melting point apparatus and are uncorrected. Flash chromatography: Merck silica gel 60 (230400 mesh) using n-hexane/ethyl acetate in various proportions as eluents unless stated
otherwise. Elemental analyses: Dornis & Kolbe, Millheim.
9
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Current Data Parameters
NAME
EXPNO
0. 3d
(A3
10/
INSTRUM
PROBWD
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TO
0
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10
0.34'
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NUCI
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4. 7C
51
mHz
-6.30 Hz
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0
-0.50 Hz
0.18
4.00
1D NMR plot parameters
DLb
9
303.0 K
1.00000000 sec
10.30 usec
4.50 usec
600.2242403 m0z
1H
0.00 dB
65536
600.2199937
SR
WDN
SSB
LB
1,0
2
12019.230 Hz
2.7263477 sec
64
41.600 usec
F2 - Processing parameters
SI
SF
5. Oil
C6D6
32
4.50 usec
DE
b4
spect
5 = TXI 13C
zg30
65536
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14
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Date
960401
Time
14.59
n
ab
10
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USER
0a
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20.00 cm
CY
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15.00 cm
6.201 ppm
Fl
3722.12 Hz
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0.495 ppm
F2
296.88 Hz
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171.26208 Hz/cm
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960403
Date_
Time
4.49
INSTRUM
spect
PROBMD 5 amTXI 13C
PULPROG
zgdc30
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65536
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50000
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8
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37593.984 Hz
0.8716788 sec
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Current Data Parameters
NAME
Igml2401
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L(I1701
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NMlE
LOMIS702
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31
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Date960424
16.19
Time
INSTRUM
&3x400
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5
32
1
0
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400.1356 MWz
2.639358 Hz
6.754 ppm
Processing parameters
512
4001343925 ftiz
5.278716 Hz
4392M4 Hz
SINE
0
0 00 Hz
0
8.00
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512
GF
400 1343925 14Hz
SINE
0
0.00 Hz
0
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ppN
PPM I
I
2702.703 Mz
1.319579 Hz
0.3789300 sec
32
185.000 usec
172.86 usec
300.0 K
5569.95 Hz
5569.95 Hz
1d
1.86692903 sec
5.60 usec
0 00000300 sec
172.86 usec
400,1355699 IMiz
1H
0 00037000sec
F1 - Acquisition perameters
40
'.3
CDC13
8
X2
CII
F2PLO
F2LO
F2PHI
F2HI
FiPLO
FILO
FIPHI
FJHI
F2PPWM
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20.00 cO
20.00 cm
b.320 pol
2528.76 Hz
-0.435 ppm
-173.94 Hz
6.320 ppa
2520.75 HZ
-0.435 ppa
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0.33772 ppm/ca
135.13515 Hz/ca
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NAME
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41
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960428
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15.09
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NAME
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512
400.1343973 MHz
SINE
0
0.00 Hz
0
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Processing parameters
512
QF
400.1343979 MHz
SINE
0
0.00 Hz
0
2D MRplot parameters
CX2
12.50 cm
Cl
12.50 cm
F2PLO
7.784 ppm
3114.79 Hz
F2LO
F2PHI
-0.383 ppm
-153 18 Hz
F2HI
7.783 ppm
F1PI0
3114.13 Hz
P100
-0.384 ppm
F1PHI
PlHI
-153 84 Hz
F2P0MCM
065338
:
ppm/cm
F2NECM
261.43790 Hz/cm
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0.65338 ppm/cm
261.43790 Hz/cm
FI1ECH
I
0
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1
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TD
256
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400.1359 MHz
FIDRES
12.765523 Hz
SW
8.167 ppm
F1
SI
MC2
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g
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F2 - Acquisition Parameters
960723
Date_
Time
13.00
INSTRUM
ax400
PROBHD 5 amMultinu
PULPROG
cosy90
TD
512
SOLVENT
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NS
8
US
4
3267-974 Hz
SOH
FIDRES
6382763 Hz
0.0783860 sec
AQ
M0
64
DK
153.000 usec
DE
152.50 usec
300.0 K
TE
1 dB
ELI
D1
2.49079393 sec
5 60 usec
P
DO
0.00000300 sec
DE
152.50 usec
400.1358781 MHz
SF11
NUCLEUS
1H
INo
0-00030600 sec
0
Current Data Parameters
19M186
13
1
NME
EXPNO
PROQ90
DU
USER
api
k1
F2 - Acquisition Parameters
960723
Date_
14.31
Time
INST0UN
a=e400
PROBD 5 m Multinu
hxco
PULPROG
TD
2048
CDC13
SOLVENT
NS
40
I4
AI
-_II-_
__o_
_-_
_
4
DS
I
*1b
-0.0
sNo
FIORS
AQ
9G
DW
DE
79
AL1
011
D1
51
-0.5
-1.0
-1.5
-2.0
ppm
PPm
50
40
30
20
10
0
P3
SF02
DECWC
DO
P2
02
P1
D3
S2
DE
SF01
NUCLIS
CPDPRG
P31
IN0
16129,032 Hz
7.875504 Hz
0 0635380sec
32768
31,000 usec
48.57 usec
300.0 K
1 dB
0.03000000 sec
3.03685809 sec
1 dB
5.40 usec
400.1358781 M3z
1H
0.00000300 sec
28.80 usec
0.00333300 se
14.40 usec
000166670 sec
29 dB
48.57 user
100.6212093 NHz
13C
waltal6
100.00 usec
0.00015300 sec
F1 - Acquisition parameters
2
NDO
TD
128
400.1359 MHz
SF01
25.531046 Hz
FIDRES
8.167 pp
SW
SI
SF
WDW
SSB
LB
GB
PC
F2 - Processing parameters
2048
100.6138650 MHz
SINE
0
0.00 Hz
0
100
SI
MC2
SF
WDW
SSB
LB
GB
F1 - Processing parameters
256
QF
400.1343918 MHz
SINE
0
0.00 Hz
0
2D NHR
plot parameters
15.00 cm
12.50 cm
58.973 ppm
5933.54 Hz
-1.455 ppm
-14635 Hz
2.566 ppa
1026.72 Hz
-0.178 ppm
-71.12 Hz
aPP0Me 4.02853 pp/m
405.32599 Hz/cm
F2HEQ(
F1PPMC1
0.21949 ppamca
FlazCM
87.82681 z/m
CX2
CX1
F2PLD
F2LO
F2PHI
P2nz
F1PLO
F10
FPPI
P182
Me3 SIO
12b
.
ppm
6
5
4
3
II
2
0
Me3 SiQ
12b
I
pprn
140
I
120o
ibo
100
80
60
I
I
40
20
I
6
I
0
Current Data7 Parameters
1gm 601
NAME
EXPNO
14
PROCNO
1
api
WS
USER
k1
0
kO
12b
0o
F2 - Acquisition Parameters
960703
Date_
1.26
Time
anx400
INSTRUM
PROBED 5 maMultinu
PULPROG cosy9o
TD
512
CDC13
SOLVENT
NS
8
4
DS
3649.635 Hz
SWH
7.128193 Hz
FIDRES
0.0701940 sec
AQ
32
MO
137.000 usec
IN
152 50 usec
DE
300.0 K
TE
18
H111
2-49897599 sec
D1
5.60 usec
P1
0.00000300 sec
00
152.50 usec
DE
SFo
400-1352048 MEE
1H
NUCLEUS
0.00027400 sec
INO
F1 - Acquisition parameters
I
NDO
256
TO
400.1352 MHz
SF01
14.256387 Hz
FIEES
9.121 ppa
SW
g
kg g
-2
00
* 60
0
ea
SI
SF
WOW
SSB
LB
PC
F2 - Processing parameters
512
400.1344023 MHz
SINE
S
0.00 Hz
8-00
0
0
0
o0
e
*0
e*
o6
0
-4
2D NMRplot parameters
Cx2
12.50o c
12.50 cm
CX1
6.406 ppm
F2PLO
2563.15 Hz
F2LO
-0.471 ppa
F2PHI
-188.34 Hz
F2HI
6.245 ppe
F1PLO
F1LO
2498.99 Hz
-0.471 ppm
F1PHI
-188.34 Hz
FlHI
0.55011 pps/ca
F2PaCM
220.11861 Hz/cm
F2HECM
0.53729 ppa/cm
F1PPMCM
214.98631 Hz/cm
Fl9CM
6
00*
*
2
ppm
ppm
4
2
0
F1 - Processing parameters
512
SI
MC2
QF
400.1344023 Maz
SF
SINE
WOW
SSB
0
0.00 Hz
LB
GB
0
Current Data Parameters
1gm17601
NAME
14
EXPNO
1
PROHO0
api
DU
USER
k1
F2 - Acquisition Parameters
960703
Date_
1.26
Time
amx400
INSTWM
Multinu
PROBED 5 mm
PULPROG
cosy90
512
TD
CDC13
SOLVENT
NS
8
4
DS
3649 635 Hz
SW
7-128193 Hz
FIDPRES
0.0701940 sec
AQ
32
HG
137.000 usec
DW
152 50 usec
DE
300,0 K
7
K
0
1 dB
HL1
-0.0
12b
DI
P1
DO
DE
SFo
NUCLEUS
INO
2.49897599 sec
5.60 usec
0.00000300 sec
152.50
usec
NHz
400.135204
1H
sec
0,00027400
F1 - Acquisition
parameters
0
-0.5
0
.
-1.0
CD..
0
To
SF01
FIDRES
Sw
SI
SF
WDW
008
LB
GB
PC
0
H
S.
-1.5
O
-2.0
O
0
-2.5
ppm
0
I
ppm
I
2.0
I
1.5
1.0
F2 - Processing
parameters
512
400.1344023 MHz
SINE
0
0.00 HZ
0
8.00
F1
0
0
0.5
1
0.0
SI
MK2
SF
WDW
SSB
LB
GB
256
MHz
400,1352
Hz
14.256387
9.121 ppm
Processing parameters
512
oF
MHz
400.1344023
SINE
H
0.00 Hz
0
2D HERplot parameters
12.50 cm
CX2
12.50 cm
CX1
F2PL0
2.593 ppu
1037.71 Hz
F2LO
F2PHI
-0.417 ppm
F291
-166.95 Hz
2.647 ppm
F1PLO
1059.10 Ez
FILO
-0.293 ppa
F1PHI
-117.06 Hz
F1HI
0.24085 ppm/cm
F2PPHCM
96.37318 Hz/cm
F2HECM
023515 pun/cm
F1PPHCM
9409216 Hz/tm
718M0
Me 3SiQ
NAME
EXPND
PROC0
Current Data Parae ters
1gim17601
15
1
api
DU
USER
k1
F2 - Acquisition Parameters
960703
Date2.56
Time
INSTRUM
a"d00
PROBBM 5m Multinu
12b
409-op swmit
I
-l-
01-0 P~ N, di
I fi 0 0 A
PULPROG
TD
SOLVENT
NS
DS
0A
hxco
2048
CDC13
32
4
31250.000 Hz
15.258789 Hz
0.0328180 sec
32768
RG
DN
16.000 usec
DE
48.57 usec
TE
300.0 x
OS1
IdB
0-03000000 sec
D11
3-01638389 sec
D1
Si
1 dB
5.40 usec
P3
MHz
400.1352048
SF02
DECNUC
1N
0.00000300 seec
DO
P2
28.80 usec
0.00333330 sec
D2
14.40 user
PI
000166670 seec
03
S2
29 dB
48.57 usec
DE
HHz
100.6256314
SF01
NUCLEUS
13C
CPDPRG
waltal6
100.00 usec
P31
0.00013700 sec
INo
SWO
FIDRES
AQ
II
-- so
NDO
Fl - Acquisition parameters
2
TD
128
SF01
FIDRES
SW
Mz
400.1352
28.512774
Hz
9.121
ppm
parameters
F2 - Processing
SI
2048
100.6138708 MHz
SF
SINE
WOW
0
SSB
0.00 Hz
LB
GB
0
PC
1.00
SI
MC2
SF
WDN
SSB
LB
GB
'A
6
ppm
m ....
2...5.....
5
100
75
25
I
Fl - Processing parameters
256
OF
4001344023 MHz
SINE
0
0O00
0
HZ
2DNNRplot parameters
15 00 cm
12.50 cm
154.196 ppm
15514.30 Hz
-15.053 pp
-1514.50 Hz
6.388 pp
lPLO
2556.02 Hz
FiLO
-S 417 Ma
FiRNI
-166.85 Kz
P181
v2PPmeN
11.2327 pa/c.
1135.25391 Hz/cm
F2Hzcx
0.54441 ppm/ca
F1PP8CH
217.83759 Hz/cm
F1EzCX
eX2
CII
F2PLO
F2LO
F2PHI
F280
Current Data Parameters
Igml7601
NAME
EXPNO
15
1
PROCN0
DU
api
USER
ki
F2 - Acquisition Parameters
960703
DateTime
2.56
INSTRUM
ax4OO
PROBD 5 mm Nultinu
.LJJNNIWLLL.
,M
IIII.II"im..I -i
10,
1 I1.
PULPROG
*wo
A
12b
-0.0
-0.5
-1.0
-1.5
-2.0
ppm
p4
ppm
50
40
1
j I, I I .I
30
20
I.I.II1I1
0
10
II1 II
0II
0
hxco
2048
CDC13
32
4
31250.000 Hz
15,258789 Hz
0.0328180 sec
32768
16 000 usec
DE
48 57 usec
TE
300.0 K
I dB
HL1
D11
0 03000000 sec
D1
3 01638389 sec
S1
1 dB
P3
5.40 user
400.1352048 Mz
SF02
1
DECNUC
0.00000300 sec
DO
28 80 usec
P2
02
0.00333330 sec
P1
14.40 usec
D3
0,00166670 sec
S2
29 d5
DE
48.57 usec
SF01
100.6256314 mmz
NUCLEUS
130
CPDPRG
waltzl6
100.00 usec
P31
INO
0.00013700 sec
TD
SOLVENT
NS
DS
SW
FIDRES
AQ
RG
WN
Fl - Acquisition parameters
NDO
2
128
TD
SF01
400.1352 MHz
FIDRES
28.512774 Hz
SW
9.121 ppe
SI
SF
WW
ss5
LB
GB
PC
SI
NC2
SF
NW
SSB
LB
F2 - Processing parameters
2048
100.6138708 MHz
SINE
0
0.00 Hz
0
1.00
P1 - Processing parameters
256
QF
400.1344023 MHz
SINE
0
0005Z
08
0
2D 8MRplot parameters
C02
15 00 cm
COO
12 50 cm
F2PLO
62.141 ppa
F20
6252.21 Hz
-3.678 ppa
F2PHI
-370.10 Hz
72n0
2.469 Dm
F1PLO
987.81 Hz
FlL
-0.168 pM
FOPOI
P1381
-67.16 Ht
P2P98~06
4.38794 ppm/cm
F2HEC8
441.48761 Hz/ca
F1PPMK
0.21092 ppa/c
FlHECK
84.39781 Hz/c
13
L
w
k"
5
4
I
32
I
I
1
13
ppm
140
120
I
100
I
I
80
60
40
II
I
20
1
pm
5.5
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5
1.0
0.5
1
. t- ji.- a i L.i.~..601L
MIIT 1r "
ppm
120
100
doIld~b..LLLJJ
r i,-i mi1,- 1i prA ~i-PEi
80
60
40
.j
M.j
jUl A
IIAM16A
iqI-I~
ii.jLjLd
~
o
d.

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