反应详情

温度

0 °C

THF (180 ml), H-Pro-OBzl.HCl (43.5 g, 0.18 M) and HOBT (24.3 g, 0.18 M) were added to BOC-Pro-OH (36.6 g, 0.17 M); DMF (100 ml) was added, and WSCI (33.0 ml, 0.18 M) was added dropwise at 0° C. After stirring at 0° C. for one hour and at room temperature overnight, the solvent was distilled off in vacuo. Benzene (500 ml) was added to the residue, which was washed three times with 5% sodium bicarbonate, three times with 1 N HCl and three times with water, in that order. After drying with anhydrous sodium sulfate, the solution was concentrated in vacuo to obtain the oily material [23] (74 g, yield: 100%).

1. additionWSCI (33.0 ml, 0.18 M) was added dropwise at 0° C
2. distillationthe solvent was distilled off in vacuo
3. additionBenzene (500 ml) was added to the residue, which
4. washwas washed three times with 5% sodium bicarbonate, three times with 1 N HCl and three times with water
5. dry with materialAfter drying with anhydrous sodium sulfate
6. concentrationthe solution was concentrated in vacuo