Methyl iodide → HCID 19956386, compound

Participants

Reaction Steps

To a solution of 0.46 g (0.73 mmol) of (E)-1-ethyl-1,5,10,14-tetra-BOC-1,5,10,14-tetraazatetradec-7-ene (see Example 5a) in 6 ml of DMF there are added, with stirring, 0.059 g (1.47 mmol) of sodium hydride dispersion (approx. 60% ) and, after 5 min., 0.092 ml (1.47 mmol) of methyl iodide. The reaction mixture is stirred for 15 h at room temperature; a further 0.029 g (0.725 mmol) of sodium hydride dispersion (approx. 60%) and 0.045 ml (0.721 mmol) of methyl 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=0.42 (silica gel/ethyl acetate:hexane (1:1)).

Provenance & Evidence