Iodoethane → HCID 19956413, compound

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Reaction Steps

To a solution of 0.272 g (0.424 mmol) of (E)-1-allyl-1,5,10,14-tetra-BOC-1,5,10,14-tetraazatetradec-7-ene (see Example 2a) in 4 ml of DMF there are added, with stirring, 0.034 g (0.85 mmol) of sodium hydride dispersion (approx. 60%) and, after 5 min., 0.069 ml (0.85 mmol) of ethyl iodide. The reaction mixture is stirred for 15 h at room temperature; a further 0.017 g (0.425 mmol) of sodium hydride dispersion (approx. 60%) and 0.034 ml (0.421 mmol) of ethyl iodide are added, and the mixture is stirred for a further 96 h at 20° C. and is then concentrated by evaporation in vacuo. Working up analogously to Example 1a), but using ethyl acetate-hexane (1:2) in the flash chromatography, yields the title compound, Rf value=0.53 (silica gel/ethyl acetate:hexane (1:1)).

Provenance & Evidence