反应详情

A solution of compound 3 (3.0 g, 14.2 mmol) in THF (10 mL) is added to a suspension of sodium hydride (60%, 0.63 g, 15.6 mmol) in THF (60 mL) at 0° C. The reaction mixture is kept at the same temperature for 2 hours and methyl iodide (0.93 mL, 14.9 mmol) is added at 0° C. The reaction mixture is allowed to warm up to room temperature overnight and then quenched with water. The mixture is separated and the aqueous phase is extracted with ethyl acetate (2×40 mL). The extracts are combined, washed with brine, dried, concentrated and purified by column chromatography (hexane/ethyl acetate 50:1 to 4:1) to give 4 (2.2 g, 69%) as a yellow solid.

1. customquenched with water
2. customThe mixture is separated
3. extractionthe aqueous phase is extracted with ethyl acetate (2×40 mL)
4. washwashed with brine
5. customdried
6. concentrationconcentrated
7. custompurified by column chromatography (hexane/ethyl acetate 50:1 to 4:1)