Methanol → HCID 131736690, Verbindung

2-Chlorotrityl chloride resin (1.07 mmol/g, 100-200 mesh, 1% DVB, manufactured by Chem-Impex, 3.00 g, 3.21 mmol) and dichloromethane (20 ml) were mixed, followed by shaking at room temperature. Dichloromethane was removed, after which methanol (0.52 ml, 12.85 mmol) and diisopropylethylamine (1.35 ml, 7.75 mmol) were added to a solution of (S)-6-(4-(2-((((9H-fluoren-9-yl)methoxy) carbonyl)amino)-3-oxo-3-(piperidin-1-yl)propyl)phenyl)hexanoic acid (Compound SP427) (0.91 g, 1.60 mmol) in dichloromethane (14 ml) and the resulting mixture was added to the resin, followed by shaking at room temperature for 5 minutes. The reaction solution was removed, after which methanol (4.2 ml) and diisopropylethylamine (1.4 ml) were added to dichloromethane (14 ml), and the resulting mixture was added, followed by shaking at room temperature for 2.5 hours. This reaction solution was removed, and dichloromethane (20 ml) was then placed, followed by shaking. Dichloromethane was removed, and dichloromethane (20 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 SP428) (3.15 g).

1. customDichloromethane was removed
2. additionthe resulting mixture was added to the resin
3. stirringby shaking at room temperature for 5 minutes
4. customThe reaction solution was removed
5. additionafter which methanol (4.2 ml) and diisopropylethylamine (1.4 ml) were added to dichloromethane (14 ml)
6. additionthe resulting mixture was added
7. stirringby shaking at room temperature for 2.5 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

ORD-Eintrag

ord-9f89edc86b9e4e9d8e21caac17d34345

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09409952B2