Triphenylphosphine → HCID 18624186, compound

Participants

Reaction Steps

A solution of diethyl azodicarboxylate (0.488 g, 2.8 mmol) in 3 ml THF was added to a solution of the product of STEP 7 (0.72 g, 2.16 mmol) and triphenylphosphine (0.734 g, 2.8 mmol) in 13 ml THF at room temperature and stirred for 15 min. Tert-butyl N-(3-hydroxypropyl) carbamate (0.491 g, 2.8 mmol) was added. The reaction was stirred at room temperature for 18 h. THF was evaporated and the residue was purified by chromatography (on silica gel, ethyl acetate/hexane=1/4) to yield a golden oil in 0.87 g. This product was dissolved in 10 ml ethanol and 10 ml 4N HCl/dioxane and stirred at room temperature for 1 h. Solvents were evaporated to afford a light golden oil in 0.734 g. NMR spectra of the product were consistent for the proposed structure.

Provenance & Evidence