反应详情

To a suspension of sodium hydride (1.1 g, 38.5 mmol) in THF (30 mL) at room temperature was added a solution of compound 20 (2.0 g, 8.37 mmol) in THF (15 mL) and the resulting reaction mixture was allowed to stir at room temperature for 1 hour. Thereafter a solution of bromo acetic acid (2.68 g, 19.25 mmol) in THF (5 mL) was added dropwise and the resulting reaction mixture was allowed to stir at room temperature for 18 hours. The reaction mixture is poured onto water and extracted with ethyl ether (3×100 mL) and the combined ethyl ether extracts were dried over anhydrous sodium sulfate and concentrated in vacuo. Chromatography (SiO2, 20 to 70% EtOAc-Hexanes eluant) provided 1.0 g of 22 as a clear oil (2.48 g, theoretical, 40% yield).

1. customthe resulting reaction mixture
2. customthe resulting reaction mixture
3. stirringto stir at room temperature for 18 hours
4. additionThe reaction mixture is poured onto water
5. extractionextracted with ethyl ether (3×100 mL)
6. dry with materialthe combined ethyl ether extracts were dried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo