反应详情

温度

0 °C

1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (443 mg) in one portion was added to a mixture of N-Boc-L-norvaline dicyclohexylammonium salt (838 mg), N,O-dimethylhydroxylamine hydrochloride (215 mg), 1-hydroxybenzotriazole monohydrate (340 mg), and N-methylmorpholine (0.28 ml) in dimethyl formamide (DMF, 20 ml) at 0° C. The mixture was stirred at 0° C. for 2 hours, then at room temperature for 40 hours. The reaction was quenched with water (80 mL) and the mixture was extracted with ethyl acetate (EtOAc, 3×100 mL). The combined organic layers were washed with aqueous 10% hydrogen chloride (HCl), saturated sodium bicarbonate (NaHCO3), and brine, then dried over anhydrous magnesium sulfate (MgSO4), filtered, and evaporated to afford the product (546 mg) as an oil.

1. waitat room temperature for 40 hours
2. customThe reaction was quenched with water (80 mL)
3. extractionthe mixture was extracted with ethyl acetate (EtOAc, 3×100 mL)
4. washThe combined organic layers were washed with aqueous 10% hydrogen chloride (HCl), saturated sodium bicarbonate (NaHCO3), and brine
5. dry with materialdried over anhydrous magnesium sulfate (MgSO4)
6. filtrationfiltered
7. customevaporated