HRID1482254

反应详情

EQUATION

反应方程式

HRID 1482254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chlorotrityl chloride resin (1.07 mmol/g, 100-200 mesh, 1% DVB, manufactured by Chem-Impex, 5.00 g, 5.35 mmol) and dichloromethane (35 ml) were placed, followed by shaking at room temperature. Dichloromethane was removed, after which methanol (0.87 ml, 21.50 mmol) and diisopropylethylamine (2.24 ml, 12.86 mmol) were added to a solution of (S)-5-(3-(2-((((9H-fluoren-9-yl)methoxy) carbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)pentanoic acid (Compound SP432) (1.48 g, 2.67 mmol) in dichloromethane (33 ml), and the resulting mixture was added to the resin, followed by shaking at room temperature for 10 minutes. The reaction solution was removed, after which methanol (10 ml) and diisopropylethylamine (3.3 ml) were added to dichloromethane (33 ml), and the resulting mixture was added, followed by shaking at room temperature for 2 hours. This reaction solution was removed, and dichloromethane (33 ml) was then placed, followed by shaking. Dichloromethane was removed, and dichloromethane (33 ml) was then placed again, followed by shaking. Dichloromethane was removed, and the resin was then dried under reduced pressure to afford the title compound (Compound SP433) (5.80 g).

WORKUP

后处理

  1. customDichloromethane was removed
  2. additionthe resulting mixture was added to the resin
  3. stirringby shaking at room temperature for 10 minutes
  4. customThe reaction solution was removed
  5. additionafter which methanol (10 ml) and diisopropylethylamine (3.3 ml) were added to dichloromethane (33 ml)
  6. additionthe resulting mixture was added
  7. stirringby shaking at room temperature for 2 hours
  8. customThis reaction solution was removed
  9. stirringby shaking
  10. customDichloromethane was removed
  11. stirringby shaking
  12. customDichloromethane was removed
  13. customthe resin was then dried under reduced pressure