Triphenylphosphine → HCID 58542327, compound

Participants

Reaction Steps

Triphenylphosphine (1.57 g, 5.99 mmol) and diisopropyl azodicarboxylate (0.93 ml, 4.49 mmol) were added to a toluene (100 ml) solution of the compound (1.26 g, 3.00 mmol) obtained in Step 3 above under ice cooling and the resulting mixture was gradually returned to room temperature while being stirred for 18 hours. Further triphenylphosphine (1.57 g, 5.99 mmol) and diisopropyl azodicarboxylate (0.93 ml, 4.49 mmol) were added and the resulting mixture was heated to reflux for 4 hours. The reaction mixture was concentrated under reduced pressure and the residue obtained was purified by silica gel column chromatography [n-hexane:ethyl acetate=3:1 (v/v)] to give the title compound (0.57 g, 47%) as a colorless oil.

Provenance & Evidence