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. 2022 Dec 23;11(12):e202200252. doi: 10.1002/open.202200252

Table 1.

Optimization of reaction conditions.[a]

graphic file with name OPEN-11-e202200252-g001.jpg

Entry

Solvent

Base/additive

3 a [%][b]

4 a [%][b]

Selectivity 3 a/4 a

1

DMAc

Cs2CO3

14

25

0.56

2

DMAc

K3PO4

27

31

0.87

3

DMAc

KOtBu

45

12

3.75

4

DMAc

NaOtBu

57

19

3.00

5

DMAc

NaH

58

6

DMAc/DMAc[c]

NaOMe

63/73

15/27

5.25/2.70

7

DMAc

K3PO4/TBACl

9

46

0.19

8

DMAc[c]

NaOMe/TBACl

7

93

0.08

[a] 1 equiv.=0.5 mmol, Atmospheric conditions unless otherwise noted. MAc=dimethylacetamide. [b] Isolated yield. [c] Argon atmosphere.