Triphenylphosphine → HCID 57137509, compound

Participants

Reaction Steps

A solution of 1.50 g (0.0088 mol) 7-hydroxy-naphthalene-2-carbonitrile, 3.93 g (0.0088 mol) 4-{4-[(diethoxy-phosphoryl)-hydroxy-methyl]-phenoxy}-piperidine-1-carboxylic acid tert.-butyl ester and 3.73 g (0.0142 mol) triphenylphosphine in 150 ml tetrahydrofuran is admixed at 5° C. with 2.23 ml (0.0142 mol) azodicarboxylic acid diethyl ester and stirred for 96 h at room temperature. After concentration the residue is purified by chromatography on a silica gel column (mobile solvent: ethyl acetate/methanol 19:1). After concentrating the appropriate column fractions one obtains 2.47 g (47%) of the title compound as a viscous, yellow oil. 31P-NMR: δ=19.0 ppm.

Provenance & Evidence