反应详情

温度

0 °C

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 3-hydroxy-2-[5-(2-methyl-[1,3]dioxolan-2-yl)-pentanoylamino]-propionic acid methyl ester (1.40 g, 4.84 mmol) in dry THF (15 mL) was added at −10° C. to a solution of (methoxycarbonylsulfamoyl)triethylammonium hydroxide (1.43 g, 5.81 mmol) in dry THF (35 mL) and the resulting suspension was stirred at 0° C. for 1.5 h. The reaction mixture was then stirred at reflux overnight. The mixture was then allowed to cool down to rt and filtered. The filtrate was concentrated under reduced pressure to give the title compound as a pale yellow oil. TLC: rf (1000:50:4 CH2Cl2-MeOH—NH3)=0.45.

1. stirringThe reaction mixture was then stirred
2. temperatureat reflux overnight
3. temperatureto cool down to rt
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure