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J. Chem. Sci.
( 2 0 1 9 ) 1 3 1 : 1 2 1
3
5
2.2c Isolation of 1ÁEtOH
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2. Experimental
1 Materials and general procedures
2.2f Synthesis of 2ÁiPr2NEt; [(iPrAr’O)2P(O)(O)]-ÁH–
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A
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2
1
3
s
p
e
c
t
r
o
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t
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r
.
3
(
N
C H CH )
2 3
p
p
m
H
}
.
N
M
R
(
1
2
K
1
B
.
4
r
4
2
p
M
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e t
z
,
,
C
c
D
C
l
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,
:
3
1
2
ꢀ
t =
5
°
C
)
:
d
=
–
,
,
1
b
2
1
.
0
,
7
m
2
)
F
T
-
I
R
(
e
l
l
m -
3
4
2
0
(
w
r
)
3
(
w
)
,
3
0
5
7
(
m
)
,
3
0
2
4
(
m
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2
9
5
7
2
.
2
S
y
n
t
h
e
s
i
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o
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4
(
s
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(
w
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3
8
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w
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9
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9
4
3
(
w
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1
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w
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8
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1
1
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3
w
8
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4
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1
5
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9
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3
m
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1
4
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9
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3
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8
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5
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s
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4
w
4
)
5
,
(
1
s
2
)
4
,
1
4
3
(
9
s )
9
,
2.2a Isolation of 1ÁDMF
S
(
l
0
o
.
w
5
e
m
v
L
a
p
)
o
r
s
a
o
t
l
i
u
o
t
n
i
o
n
f
a
(
w
(
w
6
2
(
w
(
w
1
2
d
i
m
e
t
h
y
l
f
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a
m
i
d
e
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D
M
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o
f
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2
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5
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m
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1
m
w )
1
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7
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7
7
8
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9
1
w
6
(
)
(
s
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1
1
5
8
8
9
5
(
0
( s
m
)
,
1
1
8
2
2
(
0
9
w
(
m
)
)
4
,
1
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9
8
6
3
(
(
6
s
w
2
)
,
)
8
1
0
6
w
3
3
)
1
1ÁEt2O
(
0
a
.
n
1
t
0
0
a
g
)
e
a
f
t
o
r
o
o
m
t
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m
p
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t
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e
.
l
e
a
d
s
t
o
a
n
(
m
)
,
9
2
s
)
,
(
m
)
,
(
w
,
7
,
7
a
l
m
o
s
t
q
u
i
t
t
i
v
r
m
a
t
i
o
f
1
Á
D
M
F
(
m
)
,
7
4
(
)
,
6
9
)
,
6
6
6
)
,
6
6
(
w
)
,
(
,
2.2b Isolation of 1ÁMeOH
S
l
o
w
e
(
t
v
0
i
a
p
0
o
r
a
g
t
i
o
a
o
n
o
o
t
f
a
6
0
6
(
m
)
,
5
8
0
(
w
)
,
5
1
6
(
w
)
.
C
H
3
O
H
(
5
r
m
L
)
s
o
l
t
u
o
t
t
i
o
n
o
f
1
Á
E
t
O
.
1
0
)
f
t
r
a
o
m
n
2
2.2g Synthesis of 2ÁNHCiPr2Me2
;
[(iPrAr’O)2
I n a 1 0 0 m L S c h l e n k
t
e
m
p
e
r
a
t
u
e
l
e
a
d
s
h
e
a
l
m
o
s
t
q
u
a
n
t
a
t
i
v
e
r
m
i
o
-
P(O)(O)]-ÁH–NHCiPr2Me2?
o
f
1
Á
M
e
O
H
.