反应详情

A mixture of N-Boc-L-leucine (2.47 g), N,O-dimethylhydroxylamine hydrochloride (1.09 g), 1-hydroxybenzotriazole monohydrate (1.51 g), and N-methylmorpholine (1.21 mL) was dissolved in DMF (40 mL), 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.14 g) was added at 0° C. and the mixture was stirred at 0° C. for 2h, then at room temperature for 22 h. The reaction was quenched with water (100 mL) and the mixture was extracted with EtOAc (3×100 mL). The combined organic layers were washed with aqueous 10% HCl, saturated NaHCO3, and brine, then dried over anhydrous MgSO4, filtered, and evaporated to afford the product (2.57 g) as an oil.

1. customThe reaction was quenched with water (100 mL)
2. extractionthe mixture was extracted with EtOAc (3×100 mL)
3. washThe combined organic layers were washed with aqueous 10% HCl, saturated NaHCO3, and brine
4. dry with materialdried over anhydrous MgSO4
5. filtrationfiltered
6. customevaporated