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The preparation and isolation of the metalated ylides [Cy3PCSO2Tol]M (Cy1‐M) (with M = Li, Na, K) are reported. In contrast to its triphenylphosphonium analogue the synthesis of Cy1‐M revealed to be less straight forward. Synthetic routes to the phosphonium salt precursor Cy1‐H2 via different methods revealed to be unsuccessful or low‐yielding. However, nucleophilic attack of the ylide Cy3P = CH2...
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