反应详情

A solution of dimethyl methylphosphonate (13.20 g, 106.5 mmol) in anhydrous THF (165 mL) was cooled to −78° and treated dropwise with 2.5 M n-BuLi (42.3 mL). After stirring at −78° for 45 min, a solution of ester 1-5 (6.6 g, 26.6 mmol) in THF (35 mL) was added dropwise and the resulting solution stirred for 30 min −78°, quenched with sat. NH4Cl (100 mL), then extracted with ethyl acetate (3×150 mL). The combined organic extracts were dried (MgSO4), filtered, and concentrated to afford a yellow oil. Chromatography on silica gel (5% MeOH/CH2Cl2) afforded 15-1 as a yellow oil.

1. stirringthe resulting solution stirred for 30 min −78°
2. customquenched with sat. NH4Cl (100 mL)
3. extractionextracted with ethyl acetate (3×150 mL)
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customto afford a yellow oil