反应详情

A suspension of dimethyl(2-oxopropyl)phosphonate (2.1 g, 12.9 mmol) and potassium carbonate (2.2 g, 15.9 mmol) in dry MeCN (40 mL) was treated with slow addition of a solution of 4-dodecylbenzenesulfonyl azide (5.7 g, 16.2 mmol) in dry MeCN (90 mL) for over 30 min. After being stirred for 2.5 h under N2 atmosphere at room temperature, the mixture was treated with saturated NH4Cl (100 mL), poured into a separatory funnel and extracted with EtOAc (3×100 mL), dried over Na2SO4, filtered, solvent evaporated and the residue chromatographed in a cartridge of silicagel (40 g) eluted with 15% to 100% EtOAc in hexane (UV detection at 254 nm), to afford reagent 29 as a light yellow oil.

1. additionpoured into a separatory funnel
2. extractionextracted with EtOAc (3×100 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customsolvent evaporated
6. customthe residue chromatographed in a cartridge of silicagel (40 g)
7. washeluted with 15% to 100% EtOAc in hexane (UV detection at 254 nm)