A neoglycolipid of structure β-D-Glcp-S-(CH2)3N(OH)(CH2)4-O-cholest-5-en-3β-yl has been prepared in fair overall yield by reduction of the nitrone obtained by condensation of β-D-Glcp-S-(CH2)3NHOH and OCH-(CH2)3-O-cholest-5-en-3б-yl. This synthetic procedure is very flexible, allowing a large range of lengths for the spacer arm, different positions for the NOH group along the spacer arm chain and the replacement of the sulfur by other bio-isosteric groups. The new neoglycolipid spontaneously oxidized to the corresponding nitroxide free radical whose EPR spectrum gave information on its conformational equilibrium which was further studied by molecular mechanics.