反应详情

N-methylmorpholine (0.107 mL, 0.986 mmol), TBTU (0.191 g, 0.592 mmol) and 2-(methylamino)acetamide hydrochloride (0.123 g, 0.986 mmol) were added to an ice-cooled suspension of 331e) (0.2 g, 0.493 mmol) in DMF (4 mL). The reaction mixture was stirred at room temperature for 16 h and then diluted with ice-cold water. A precipitate was filtered off and dissolved in dichloromethane. The organic phase was washed with sodium hydrogen carbonate solution (20 mL) and brine (20 mL), dried over sodium sulfate and evaporated. The remnant was purified by flash column chromatography [silica gel; dichloromethane with 4% methanol] followed by preparative HPLC. White solid. Yield: 65 mg (28% of theory)

1. temperaturecooled
2. additiondiluted with ice-cold water
3. filtrationA precipitate was filtered off
4. dissolutiondissolved in dichloromethane
5. washThe organic phase was washed with sodium hydrogen carbonate solution (20 mL) and brine (20 mL)
6. dry with materialdried over sodium sulfate
7. customevaporated
8. customThe remnant was purified by flash column chromatography [silica gel; dichloromethane with 4% methanol]