反应详情

温度

50 °C

Compound 136 (150 mg, 0.555 mmol) was dissolved in DMF (2.5 mL), and 2-hydroxy-2-methylpropanoic acid (116 mg, 1.11 mmol), EDC hydrochloride (313 mg, 1.11 mmol) and 1-hydroxybenzotriazole monohydrate (170 mg, 1.11 mmol) were added thereto, followed by stirring at 50° C. for 3 hours. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and then the solvent was distilled away under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=1:1) to afford the entitled Compound 137 (158 mg, 80%).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled away under reduced pressure
5. customThe resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=1:1)