反应详情

温度

19 °C

4-Methylmorpholine (2.53 g, 25 mmol) was added to a solution of H-Lys(Z)-Leu-Leu-OMe·HCl (13.93 g, 25 mmol) in DMF (85.0 g) at 10° C. HOBt (3.38 g, 25 mmol), Boc-Leu-Leu-OH (8.61 g, 25 mmol) and DIC (3.47 g, 27.5 mmol) were added over 30 min at 8-10° C. An additional portion of DMF (5.0 g) was added and the reaction was kept at 8-10° C. for 16 h. The reaction was stirred at 18-20° C. for 3 h, cooled to 5-10° C. and treated with H2O (130.0 g). A solid precipitated at 25° C. which was filtered, washed with H2O and recrystallized from MeOH and H2O to give Boc-Leu-Leu-Lys(Z)-Leu-Leu-OMe (SEQ. ID No. 2) (18.3 g, 86.4%).

1. temperaturecooled to 5-10° C.
2. customA solid precipitated at 25° C. which
3. filtrationwas filtered
4. washwashed with H2O
5. customrecrystallized from MeOH and H2O