反应详情

温度

60 °C

To a solution of ethyl 3-amino-3-methylbutyrate hydrochloride (333 mg) in tetrahydrofuran (4.00 mL), a solution in tetrahydrofuran (2.00 mL) of the compound (100 mg) obtained in step (2) above and potassium carbonate (406 mg) were added and the mixture was stirred at 60° C. for three days. After passing the reaction mixture through Celite (registered trademark), the filtrate was concentrated under reduced pressure and the resulting residue was roughly purified by preparative HPLC. To the resulting roughly purified product, a saturated aqueous solution of sodium hydrogencarbonate was added and extraction was conducted with chloroform. The combined organic layers were dried over anhydrous magnesium sulfate and after removing the desiccant by filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=98:2-50:50) to give the titled compound as a colorless amorphous mass.

1. concentrationthe filtrate was concentrated under reduced pressure
2. customthe resulting residue was roughly purified by preparative HPLC
3. additionTo the resulting roughly purified product, a saturated aqueous solution of sodium hydrogencarbonate was added
4. extractionextraction
5. dry with materialThe combined organic layers were dried over anhydrous magnesium sulfate
6. customafter removing the
7. filtrationdesiccant by filtration
8. concentrationthe filtrate was concentrated under reduced pressure
9. customThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=98:2-50:50)