Azide-armed α-1-C-alkyl-imino-d-xylitol derivatives have been efficiently prepared by way of olefin cross-metathesis in eight to nine steps and in an overall yield of 19% to 26% from 2, 3, 4-tri-O-benzyl-d-xylopyranose. Optimization of cleavage conditions of N-NAP-protected tertiary amines using DDQ in CH2Cl2-H2O (18: 1) is also reported. The iminosugars synthesized will be used as key building blocks in the synthesis of multivalent iminosugars ...