تفاعل #1569426

معادلة التفاعل

methanol

diisopropylethylamine

(S)-4-(3-(2-((((9H-fluoren-9-yl)methoxy)carbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)pent-4-enoic acid

2-Chlorotrityl chloride resin

→

title compound

(S)-4-(3-(2-((((9H-fluoren-9-yl)methoxy) carbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)pent-4-enoic acid 2-chlorotrityl resin

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىDichloromethane was removed
2. 2
   workup.ADDITIONthe resulting mixture was added to the resin
3. 3
   workup.STIRRINGby shaking at room temperature for 10 minutes
4. 4
   أخرىThe reaction solution was removed
5. 5
   workup.ADDITIONafter which methanol (5 ml) and diisopropylethylamine (1.7 ml) were added to dichloromethane (16.5 ml)
6. 6
   workup.ADDITIONthe resulting mixture was added
7. 7
   workup.STIRRINGby shaking at room temperature for 2 hours
8. 8
   أخرىThis reaction solution was removed
9. 9
   workup.STIRRINGby shaking
10. 10
    أخرىDichloromethane was removed
11. 11
    workup.STIRRINGby shaking
12. 12
    أخرىDichloromethane was removed
13. 13
    أخرىthe resin was then dried under reduced pressure

الإجراء التجريبي

2-Chlorotrityl chloride resin (1.07 mmol/g, 100-200 mesh, 1% DVB, manufactured by Chem-Impex, 2.50 g, 2.68 mmol) and dichloromethane (18 ml) were mixed, followed by shaking at room temperature for 5 minutes. Dichloromethane was removed, after which methanol (0.43 ml, 10.7 mmol) and diisopropylethylamine (1.1 ml, 6.32 mmol) were added to a solution of (S)-4-(3-(2-((((9H-fluoren-9-yl)methoxy)carbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)pent-4-enoic acid (Compound SP421) (0.74 g, 1.34 mmol) in dichloromethane (16.5 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 (5 ml) and diisopropylethylamine (1.7 ml) were added to dichloromethane (16.5 ml), and the resulting mixture was added, followed by shaking at room temperature for 2 hours. This reaction solution was removed, and dichloromethane (18 ml) was then placed, followed by shaking. Dichloromethane was removed, and dichloromethane (18 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 SP422 (2.52 g).

المصدر