Aerobic oxidation of alcohols
783
solution was transferred to a 25-mL Teflon-lined 316L stainless-steel autoclave
equipped with a magnetic stirring. After the autoclave was closed, oxygen was
charged to 0.15 MPa. The autoclave was put into an oil bath that was preheated to
75 °C for 1 h. The autoclave was cooled to room temperature and carefully
depressurized. Then, 0.1 mL of the reaction mixture was transferred to a fresh
10-mL A-grade volumetric flask and diluted to volume. This final solution was then
immediately analyzed.
O2-uptake kinetics for the CuBr/NHPI system
A typical reaction was conducted as follows. Phenylethanol (5 mmol), CuBr
(0.25 mmol), and 10 mL of ethyl acetate were added to the 150-mL Teflon-lined
316L stainless-steel autoclave. The autoclave was attached to an apparatus with a
pressure transducer designed to measure the O2 pressure. The air in the autoclave
was exchanged ten times with O2, and then filled with O2 to 0.15 MPa. The
autoclave was put into a water bath that was preheated to 75 °C. When the pressure
stabilized in the apparatus, 0.5 mmol of NHPI in 5 mL of ethyl acetate was added
via a syringe through a septum. The mmol of oxygen that reacted was calculated
using volume, actual temperature, and pressure from the ideal gas equation.
Acknowledgments We gratefully acknowledge financial support from the National Natural Science
Foundation of China (No. 20643006), the Scientific Research Foundation for the Returned Overseas
Chinese Scholars, State Education Ministry and the National Basic Research Program of China
(2009CB623505).
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