反应详情

A solution of diethyl azodicarboxylate (174 mg, 1.0 mmol) in 3 ml THF was added to a solution of the product of STEP 6 (18 mg, 0.676 mmol) and triphenylphosphine (262 mg, 1.0 mmol) in 7 ml THF at room temperature and stirred for 15 min. 2-(3-Hydroxypropylamino)pyridine N-oxide (168 mg, 1.0 mmol) was added. The reaction was stirred at room temperature for 18 h. THF was evaporated and the residue purified by chromatography (on silica gel, C2HC2I/CH3OH/NH4OH=97.5/2/0.5) to afford a pale brown oil in 81.5 mg). NMR spectra of the product were consistent for the proposed structure.

1. stirringThe reaction was stirred at room temperature for 18 h
2. customTHF was evaporated
3. customthe residue purified by chromatography (on silica gel, C2HC2I/CH3OH/NH4OH=97.5/2/0.5)
4. customto afford a pale brown oil in 81.5 mg)