反应详情

To a suspension of NaH (1.30 g, 32.64 mmol, 60% in mineral oil) in THF (15 mL) under nitrogen atmosphere was added N-hydroxy-acetamidine (2.62 g, 35.4 mmol) and stirred for 1 h at room temperature. The bromo ester 3 (8 g, 27.2 mmol) in THF (2 mL) was added and refluxed for 12 h. The reaction mixture was quenched by adding brine, extracted with ethylacetate (100 mL) and dried over anhydrous Na2SO4. The organic layer was concentrated under reduced pressure and purified by flash chromatography using 25% ethylacetate in hexane as mobile phase to furnish 4 (2.8 g, 35%) as pale yellow solid, mp=200.1-202.4° C.

1. temperaturerefluxed for 12 h
2. customThe reaction mixture was quenched
3. additionby adding brine
4. extractionextracted with ethylacetate (100 mL)
5. dry with materialdried over anhydrous Na2SO4
6. concentrationThe organic layer was concentrated under reduced pressure
7. custompurified by flash chromatography