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In this Letter we describe a catalytic procedure for the diastereoselective synthesis of β-lactones bearing up to three stereogenic centers, from disubstituted ketenes and chiral β-oxyaldehydes. Tri-n-butylphosphine was determined to be the best catalyst with yields of up to 95% and moderate to good diastereoselectivity (dr up to 4:1) obtained in the formation of highly substituted β-lactones.
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