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. 2023 Jun 16;14(28):7637–7641. doi: 10.1039/d3sc02402d

Optimization of reaction conditionsa.

graphic file with name d3sc02402d-u1.jpg
Entrya Variation from standard conditions Yieldb
1 None 99%c (97%)
2 Mn instead of Zn n.o.
3 Fe instead of Zn n.o.
4 Toluene instead of MeCN <5%
5 No catalyst n.o.
6 No ligand Trace
7 Pd(TFA)2 instead of Pd(OAc)2 94%
8 Xantphos instead of DPPP 31%
9 Ni(acac)2 + L1 as catalyst n.o.
10 CuI + L1 as catalyst n.o.
11 1 bar CO 91%
a

Reaction conditions: 1a (0.2 mmol), 2a (0.3 mmol), CO (10 bar), Pd(OAc)2 (1 mol%), DPPP (1 mol%), Zn (0.3 mmol) in MeCN (2 mL) at 80 °C for 20 h.

b

Yields were determined by GC-FID analysis using n-dodecane as the internal standard.

c

Yield of the isolated product. n.o. = not observed.