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H
N
N
O
CO 2 R
O
R 3
R 4 C 6 H 4 B(OH) 2
Pd(dppf)Cl 2 , K 2 CO 3
μ
O
R 1
R 3
O
HN c -C 6 H 11
R 1
R 3
O
HN c -C 6 H 11
R 1
N
c -C 6 H 11
N
H
N
N
W 150 o C, 20 mi n
AcCl, MeO H
F-SPE
53-96%
BocHN
O
O
O
F-SPE
15-49%
R 2
30
31
32
OSO 2 C 8 F 17
R 2
R 2
C 8 F 17 O 2 SO
R 4
H 2 N
CO 2 R
29
MeOH
R 3
F-SPE
52-99%
NC
R 2
NHBoc
R 1
C 8 F 17 O 2 SO
CHO
OH
25
O
MeOH
R 4- NC
R 4
F-SPE
R 5 -NH 2
52-99%
R 2
R 2
OSO 2 C 8 F 17
R 4 C 6 H 4 B(OH) 2
Pd(dppf)Cl 2 , K 2 CO 3
μ
R 5
O
O
R 1
O
R 4
N
TFA-MeOH
H
W 150°C, 20 min
F-SPE
20-69%
HN
HN
R 5
R 5
N
N
BocHN
O
μ
W 150°C, 20 min
F-SPE
31-97%
O
O
R 2
R 1
33
34
35
OSO 2 C 8 F 17
R 1
SCHEME 10.7 Ugi reaction-based synthesis of 1,4-benzodiazepine-2,5-diones.
sequence on 33 was different from that of 30 . The amino group attached to the amide
group instead of the ester group formed 1,4-benzodiazepine-2,5-diones 34 and led to
the formation of products 35 after the Suzuki linker cleavage reactions.
Zhang and coworkers recently employed fluorous benzaldehydes in the
synthesis of tetrasubstituted furans (Scheme 10.8) [36].
-Unsaturated ketones
36 were prepared by condensation of fluorous benzaldehydes 25 and acetophenones.
Mn(OAc) 3 - and Cu(OAc) 2 -promoted cycloaddition of 36 with 1,3-diketones under
a
,
b
O
10% NaOH
EtOH
O
O
O
CHO
R 3
R 1
R 2
R 2
R 1
15-30°C , 4 h
F-SPE
Mn(OAc) 3, Cu(OAc) 2
OSO 2 C 8 F 17
OSO 2 C 8 F 17
μ
W 165°C, 25 min
25
36
F-SPE
75-90%
76-85%
B(OH) 2
R 1
R 2
O
R 4
COR 3
R 4
Pd(dppf)Cl 2 , Cs 2 CO 3
O
μ
W 130°C, 30 min
R 1
R 2
38
57-73%
O
COR 3
R 1
R 2
C 8 F 17 O 2 SO
O
O
NH 2
R 4
CO 2 R 3
37
NH
Pd(dba) 3 , JohnPhos
DBU, PhMe
O
R 4
39
μ
W 130°C, 30 min
45-69%
SCHEME 10.8 Fluorous benzaldehydes for the synthesis of tetrasubstituted furans.
 
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