反应详情

温度

-13.5 °C

A solution of HCl (28 g, 770 mmol) in ethyl acetate (100 g) at -10° C. was rapidly added to Boc-Lys(Z)-Leu-Leu-OMe (35.0 g, 55.74 mmol) under N2 at -15 to -12° C. The mixture was stirred and maintained at -15 to -12° C. for 60 to 70 min and allowed to crystallize for 1 h at -10 to -5° C. The solid was filtered while excluding moisture, washed with several portions of t-butyl methyl ether and dried in vacuo to give H-Lys(Z)-Leu-Leu-OMe·HCl (28.7 g, 91.4%).

1. customto crystallize for 1 h at -10 to -5° C
2. filtrationThe solid was filtered
3. washwashed with several portions of t-butyl methyl ether
4. customdried in vacuo