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Sly1 en01 etlici (4.5 nirnol) was dissolved in henzene (8 mL) in a quartz tuhe. The irted (300 nm: light source: Rayonet R P R 3000) and a solution of [I iiig. 1.5 mmol. 152 ILL) in henzene ( 2 mL) was slo\rly added to the rc:iction mixtiirc hy ii syringe (within cii. 2 h). As soon as the aldehyde was fully con'iiiined (TLCJ llie irsxli~ition was slopped and the solvent ecaporated i n v~icuo. The dinstcrconicric tiitlo was detemiincd hy GLC' m d ' H N M R iinnlyses. Escccs s l y 1 e n d ethcr and the desired oxetanc were obtained by coluinn chromatography (ilasli c1iroinatogr;ipliy: eluent. cyc1ohexane;ethyl acetate as ii gradient 200:l + 95, 5 ) . boi-oset;ine\ m -2d.riic~3d and ru(.-2f;ru~3f ii complcte separation of diii-\tcrcoi~umci-\ uiis posiblc. In the other eximples only ;in enrichment of the major diwtercoiwmera could he ~h i e v e d .

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The degree of association of phenyllithium is decisively influenced by solvation. Thus far it has only been known as a dimer and tetramer with ether and tetramethylethylene‐diamine as ligands. The stabilization of monomeric phenyllithium with the tridentate ligand pentamethyldiethylenetriamine has now been achieved.