反应详情

温度

-12.5 °C

A cooled solution (-15° C.) of gaseous HCl (50.0 g, 1.37 mol) in ethyl acetate (250 g) was added to Boc-Leu-Leu-Lys(Z)-OBzl (50.0 g, 71.7 mmol) at -15 to -10° C. over 15 min. The mixture was stirred at -15 to -10° C. for 75 min and t-butyl methyl ether (310 g) was added over 25 min. The temperature was allowed to rise to about -8 to -5° C. and the excess HCl was removed under reduced pressure. Another portion of t-butyl methyl ether (310.0 g) was added over 15 min and the reaction temperature was maintained at -5° C. for approximately 2 h. The resulting solid product, H-Leu-Leu-Lys(Z)-OBzl·HCl was filtered and rinsed with t-butyl methyl ether then dried to give 41.8 g, 92.1%.

1. customto rise to about -8 to -5° C.
2. customthe excess HCl was removed under reduced pressure
3. additionAnother portion of t-butyl methyl ether (310.0 g) was added over 15 min
4. temperaturethe reaction temperature was maintained at -5° C. for approximately 2 h
5. filtrationThe resulting solid product, H-Leu-Leu-Lys(Z)-OBzl·HCl was filtered
6. washrinsed with t-butyl methyl ether
7. customthen dried
8. customto give 41.8 g, 92.1%