Journal
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
Volume 142, Issue 47, Pages 19889-19894Publisher
AMER CHEMICAL SOC
DOI: 10.1021/jacs.0c10403
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Funding
- JSPS KAKENHI [JP18H05517, JP19H00897, JP20K05534, JP17K05823]
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The reductive coupling of carbon monoxide (CO) by metal hydrides is of fundamental interest and practical importance. Herein we report an unprecedented hydrodeoxygenative cyclotetramerization of CO by a trinuclear titanium polyhydride complex [(C5Me4SiMe3)Ti](3)(mu(3)-H)(mu(2)-H)(6) (1). The reaction of CO with 1 at -78 degrees C gave an ethen-1,2-diyl species [CH=CH](2-) through the hydrodeoxygenative dimerization of two molecules of CO, which upon cycloaddition to another two molecules of CO afforded a cyclobuten-3,4-diyl-1,2-diolate unit [C4H2O2](4-). The hydrogenolysis of the [C4H2O2](4-) species with H-2 yielded a tetrahydrocyclobuten-1,2-diolate species [C4H4O2](2-), which on heating at 100 degrees C gave a cyclobuten-2-yl-1-olate product [C4H4O](2-). The acidolysis of the [C4H2O2](4-) and [C4H4O](2-) species with HCl afforded gamma-butyrolactone and cyclobutanone, respectively.
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