反応 #1726657

反応方程式

DIPC

camptothecin

N,N-Bis CBZ-Lysine

→

CBZ-Lys

溶媒

methylene chloride

反応条件

後処理

1. 1
   洗浄The solution was washed with 0.1 N HCl
2. 2
   その他dried
3. 3
   その他evaporated under reduced pressure
4. 4
   その他to yield a light yellow solid, which
5. 5
   その他was recrystallized from methanol

実験手順

N,N-Bis CBZ-Lysine (311 mg, 0.75 mmol) was dissolved in 56 mL of anhydrous methylene chloride at room temperature. To this solution were added DIPC (0.12 mL, 0.75 mmol), DMAP (0.61 mg, 0.5 mmol) and camptothecin (0.087 g, 0.25 mmol) at 0° C. The reaction mixture was allowed to warm to room temperature and left for 16 h. The solution was washed with 0.1 N HCl, dried and evaporated under reduced pressure to yield a light yellow solid, which was recrystallized from methanol to give camptothecin-20-ester of N,N-Bis CBZ-Lys 13. Purification of 13 was satisfactory based on TLC and HPLC analysis.

出典