反应详情

温度

40 °C

To a solution of 558 mg (1.67 mmol) of 2J in 25 mL of 1,2 dichloroethane was added 435 mg (4.34 mmol) of succinic anhydride, 280 μL (2 mmol) of triethylamine and 112 mg (0.91 mmol) of 4-DMAP. The reaction mixture was allowed to stir at 40° C. under argon atmosphere for 2.5 hours. It was then diluted with 50 mL of ethyl acetate and washed with 3×30 mL of 5% ammonium chloride solution. The organic layer was dried (anhydrous Na2SO4) and concentrated under reduced pressure to dryness. The residue was purified by silica gel column chromatography to give 629 mg (1.45 mmol, 86%) of 2K as a colorless gum (M+H, 433).

1. washwashed with 3×30 mL of 5% ammonium chloride solution
2. dry with materialThe organic layer was dried (anhydrous Na2SO4)
3. concentrationconcentrated under reduced pressure to dryness
4. customThe residue was purified by silica gel column chromatography