General Procedure for Synthesis of Symmetric Biaryl Ketones from
Aryl hydrazine hydrochloride:
In a 100 mL reactor the mixture of aryl hydrazine hydrochloride (1
mmol), PdCl2(PPh3)2 (2
mol%) and CuI (5 mol%) and Na2CO3 (2
equiv.), in acetonitrile (10 mL) were added and pressurized with 4 bar
CO/O2 in a ratio of (3/1). This reaction mixture was
heated at 100 °C with constant stirring for 12 h. After the reaction,
the reactor was cooled at room temperature, and remained gas was vented
carefully. The reaction mixture was diluted with ethyl acetate (10 mL)
and then washed with water. The organic layer fraction was dried over
sodium sulphate and concentrated under rotary evaporation. Then obtained
crude residue was monitored by GC-MS, and purified by column
chromatography (pet ether: ethyl acetate, 80/20 v/v). The desired
product was separated by chromatography and confirmed by GC-MS, and NMR
techniques.
Supporting Information
The supporting information for this article is available on the WWW
under https://doi.org/10.1002/cjoc.2021xxxxx.
Acknowledgment
Y. A. K. gratefully acknowledges the University Grants Commission (UGC)
(New Delhi, India, for the Senior Research Fellowship (SRF).
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